Heterogeneous catalysts with controllable interface structures are of great importance to demonstrate the relationship between structure and property. Herein, magnetic Nitrogen‐doped carbon microtubes with Co nanoparticles (Fe3O4@C−Co) were prepared, which could be used for the reduction of 4‐nitrophenol(4‐NP). In the process, MoO3@FeOOH core‐shell structure was fabricated, then ZIF‐67 was decorated on the MoO3@FeOOH. After adding 2‐methylimidazole, MoO3 microrods were removed. Then the prepared FeOOH@ZIF‐67 microtubes are converted to Fe3O4@C−Co hybrid microtubes through pyrolysis. Due to the unique structures, the obtained Fe3O4@C−Co composites improved the dispersion of Co nanoparticles (NPs), diminished Co leaching, and promoted catalytic activity. The plentiful nitrogen improved electronic conductivity and brought additional active sites. The resulting Fe3O4@C−Co implies outstanding catalytic ability towards the reduction of 4‐NP. The synergistic effect between the hollow microtube and the fine dispersed Co NPs within Fe3O4@C−Co offered an excellent catalytic efficiency. More particularly, this achievement opens a new avenue to the targeted design of well‐defined nanocatalysts for practical applications in environmental remediation.

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Metallic nickel is of particular interest because of its low cost, magnetic property, and multifunctional uses. Herein, a facile strategy to fabricate one dimensional(1D) carbon microrods with magnetic Ni nanoparticles(NPs) by one‐step carbonization of nickel‐ion‐nitrilotriacetic acid coordination polymer microrods (Ni‐NTA) has been presented. After the carbonization, the original morphology of Ni‐NTA microrods is preserved well. Fine magnetic Ni NPs are well dispersed in the carbon matrix, which possesses an impressive saturation capacity for Histidine‐rich protein, BHb. Moreover, such N‐doped carbon microrods with well‐dispersed Ni NPs on its surface present an excellent catalytic performance and stability by using the reduction of 4‐nitrophenol as a model reaction. Notably, the selected Ni‐NTA microrods and melamine act as Ni‐precursor and N‐doped carbon sources play a vital role in the formation of 3D hierarchical carbon dendrites composed of carbon microfiber trunks and carbon nanotube branches.