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The preparation of carbon nitride nanotubes has proved extremely difficult—to date only small quantities of nitrogen (≤5%) have been incorporated into carbon nanotubes or filaments and the synthesis of crystalline C3N4 and CN nanotubes with their interesting predicted properties remains a challenge for the future. Now the generation of aligned C13Nx (x ≤ 1) nanofibers in high yield by pyrolyzing melamine over laser‐patterned thin films of Fe and Ni catalyst deposited on a silica substrate is reported. The resulting aligned, hollow, thin‐walled fibers exhibit unusual graphitic corrugated morphologies. The authors suggest that pyrolysis of organic precursors containing N (e.g., melamine) may provide an additional route to CN nanostructures.

We report a high-yield route to two-dimensional arrays (<400×400 μm2) of aligned C49Nx (x⩽1) nanofibers (<100 nm o.d.; <60 μm length), by pyrolyzing mixtures of ferrocene and melamine at 950–1050 °C under an Ar flow. The fibers exhibit unusual interlinked stacked-cone morphologies, ascribed to the presence of nitrogen. High-resolution electron energy-loss spectroscopy of the individual fibers reveals a 2% nitrogen content with ionization energies mainly at ∼400.9 eV, corresponding to N bonded to three C atoms within a hexagonal framework. The nanofibers may be useful for the economic fabrication of field emission sources and robust composites.