Heteroatom-doped porous carbon materials have recently attracted significant attention due to their superior catalytic activities for an oxygen reduction reaction (ORR). Transition metals co-doped with heteroatom are considered to have positive effects on improving ORR catalytic activity and stability. We report a series of novel Fe, Co incorporated in P-doped carbon materials, which give high ORR performance by an in-situ carbonization method. The ratios of the two metals and the carbonization temperatures are the key factors for the electrocatalytic activity. Due to the synergistic effect of the two transition metals, the Fe, Co incorporated in P-doped porous carbon sample, carbonized at 900 • C, shows the highest catalytic activity and stability. Electrochemical measurements show that Fe, Co incorporated in P-doped porous carbon materials are promising electrocatalysts to substitute Pt-based catalysts for fuel cells application. With the increasing environmental pollution caused by the use of fossil fuels, it is of great urgency to develop renewable energy conversion and storage devices, such as fuel cells and metal-air batteries, which are beneficial to environmental protection. The disadvantage of the present technologies is due to the sluggish oxygen reduction reaction (ORR) kinetics at the cathode, which consequently limits the working efficiency of these devices, thereby creating a need for extra ORR catalysts to increase the reaction rate. The most popular and efficient ORR catalyst is the commercial Pt/C (Pt nanoparticles loading on the carbon (XC-72)). However, due to its expensive cost, poor durability, and CO poisoning in the reaction, 1-5 the need to explore new efficient, durable, and cheap catalysts to substitute the Pt/C is urgent. In past decades, several alternatives have been developed, such as noble metal-based nanoparticles, 5,6 non-noble metal catalysts, 7,8 and metal-free materials. 9 Heteroatom-doped carbon materials are the representatives of the metal-free materials and the mechanism of the reduction of oxygen has been widely investigated. There is a consensus that the pyridine-like N and graphite-like N (also called quaternary N) are more active than the pyrrole-type N in the N-doped carbon materials for ORR. 10,11 In general, the excellent ORR catalytic activity is ascribed to the heteroatom-doped carbon material increasing the asymmetry of the carbon atomic spin density in accordance with the theoretical calculations.12,13 In 2013, Masa et al. verified that the trace amount of transition metal with heteroatom co-doped in carbon materials significantly improve the catalyst activity.14 The meticulous research showed that transition metal-doped carbon would intensify the asymmetry of the carbon atomic spin density to promote ORR. 14,15 Thus, designing transition metal-heteroatom-C electrocatalysts is applicable to improving the ORR catalytic activity. For example, Mu et al. synthesized a novel three-dimensions (3D) Fe-N-nanocarbon intercalated graphene catalyst, which possesses a high ...