The study focuses on investigating the synthesis, characterization, and performance of NiTiO3/TiO2 nanocomposites for solar hydrogen production. A heterojunction photocatalyst consisting of 99.2% NiTiO3 and 0.8% anatase TiO2 was developed using a sol-gel method. Various characterization techniques confirmed the formation of an intimate heterojunction between the two materials, leading to improved optical and electronic properties. The nanocomposite exhibited enhanced light absorption, reduced charge carrier recombination, and efficient charge separation at the interface, resulting in a 17.1% increase in hydrogen evolution rate under UV irradiation. The research underscores the potential of NiTiO3/TiO2 nanocomposites as efficient photocatalysts for solar hydrogen production, offering advancements in renewable energy applications and contributing to the development of innovative materials in the field of nanotechnology.