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A key challenge in the development of sustainable water-splitting (WS) systems is the formulation of electrodes by efficient combinations of electrocatalyst and binder materials. Cellulose, a biopolymer, can be considered an excellent dispersing agent and binder that can replace high-cost synthetic polymers to construct low-cost electrodes. Herein, a novel electrocatalyst was fabricated by combining Fe2O3 and Ni on microcrystalline cellulose (MCC) without the use of any additional binder. Structural characterization techniques confirmed the formation of the Fe2O3–Ni nanocomposite. Microstructural studies confirmed the homogeneity of the ~50 nm-sized Fe2O3–Ni on MCC. The WS performance, which involves the hydrogen evolution reaction (HER) and the oxygen evolution reaction (OER), was evaluated using a 1 M KOH electrolyte solution. The Fe2O3–Ni nanocomposite on MCC displayed an efficient performance toward lowering the overpotential in both the HER (163 mV @ 10 mA cm−2) and OER (360 mV @ 10 mA cm−2). These results demonstrate that MCC facilitated the cohesive binding of electrocatalyst materials and attachment to the substrate surface. In the future, modified cellulose-based structures (such as functionalized gels and those dissolved in various media) can be used as efficient binder materials and alternative options for preparing electrodes for WS applications. [ABSTRACT FROM AUTHOR]