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A simple catalytic CVD method for the synthesis of N-doped carbon nanocoils (CNCs), using acetonitrile as both the carbon and nitrogen source, is developed. A Ni–Fe layered double hydroxide that has not been subjected to any prior annealing or reducing treatment is used as a catalyst precursor. The steps of precursor-to-catalyst transformation, catalyst activation, deposition of CNCs, and nitrogen doping are performed in situ, in a single process.