NiCo2S4 is an important bimetallic spinel‐type sulfide that is typically synthesized using a two‐step method, which commonly involves water as a reaction medium. Here, we show that highly crystalline and high surface area NiCo2S4 could be synthesized into a nanoflake‐entangled shape. Control of solution pH under a hydrothermal condition affects the compositions and morphologies of products. It reveals that the pKas of two transition metal ions and l‐cysteine (l‐Cys) play a crucial role in the formation of NiCo2S4. Various spectroscopic analyses were performed to characterize these products, including X‐ray diffraction, energy‐dispersive X‐ray spectroscopy, gas sorption, scanning electron microscopy, transmission electron microscopy, and X‐ray photoelectron spectroscopy.

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