This study investigates the use of two-dimensional (2D) SnS to enhance the electrocatalytic performance of NiFe-layered double hydroxides (NiFe-LDH) for water splitting. The researchers synthesized a NiFe-LDH/SnS heterojunction using a hydrothermal method, which improved the conductivity and electronic environment of the NiFe-LDH sheets. The addition of SnS reduced the charge transfer resistance and modulated the electronic environment around the active sites, favoring the adsorption of intermediates during the oxygen evolution reaction (OER). Density functional theory (DFT) calculations confirmed that the NiFe-LDH/SnS heterostructure lowered the energy barriers in the conversion steps of *OH → *O → *OOH, enhancing the OER kinetics. The resulting electrocatalyst exhibited a 20% and 27% reduction in overpotential and Tafel slope compared to pristine NiFe-LDH, respectively. This work provides a strategy for enhancing the efficiency of water-splitting reactions using 2D materials to tailor NiFe-based electrocatalysts.This study investigates the use of two-dimensional (2D) SnS to enhance the electrocatalytic performance of NiFe-layered double hydroxides (NiFe-LDH) for water splitting. The researchers synthesized a NiFe-LDH/SnS heterojunction using a hydrothermal method, which improved the conductivity and electronic environment of the NiFe-LDH sheets. The addition of SnS reduced the charge transfer resistance and modulated the electronic environment around the active sites, favoring the adsorption of intermediates during the oxygen evolution reaction (OER). Density functional theory (DFT) calculations confirmed that the NiFe-LDH/SnS heterostructure lowered the energy barriers in the conversion steps of *OH → *O → *OOH, enhancing the OER kinetics. The resulting electrocatalyst exhibited a 20% and 27% reduction in overpotential and Tafel slope compared to pristine NiFe-LDH, respectively. This work provides a strategy for enhancing the efficiency of water-splitting reactions using 2D materials to tailor NiFe-based electrocatalysts.