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Novel chain‐like CoNi alloy assemblies with a length of up to 6–7 μm were successfully prepared by a surfactant‐assisted hydrothermal synthetic route at 100 °C for 2 h. The individual submicrospheres built from smaller CoNi nanoparticles had a diameter of about 400–500 nm. These microspheres were then integrated to form the novel chain‐like CoNi alloy assemblies. The effects of synthetic parameters such as surfactant and solvent on the formation and morphology of CoNi samples were investigated. The experimental results showed that N₂H₄·H₂O and CTA⁺ play important roles in the formation of the novel chain‐like CoNi alloy assemblies. Based on the structural information provided by X‐ray powder diffraction, scanning electron microscopy, transmission electron microscopy, selected‐area electron diffraction and energy‐dispersive X‐ray analysis, a growth mechanism was tentatively proposed for the …