This investigation reports synthesis of core-shell NiFe 2 O 4 /Y 2 O 3 nanoparticles by sol-gel technique and their H 2 volume generation ability via thermochemical water-splitting reaction at 900 C-1100 C. Thermochemical water-splitting process involves a cyclic operation of a low-temperature water-splitting step and relatively high temperature regeneration step using redox materials. Because of the cyclic nature of the process, the redox materials undergo thermal fatigue leading to grain growth or sintering, consequently, steady H 2 production is not realized in multiple thermochemical cycles. In this study, attempts were made to achieve steady H 2 volume generation in multiple thermochemical cycles using core-shell nanoparticles, which were synthesized using precursors such as NiCl 2 , FeCl 2 , and YCl 3 , and pluronic P123 surfactant template. H 2 volume generated by NiFe 2 O 4 /Y 2 O 3 core-shell nanoparticles was found to be relatively stable over multiple thermochemical cycles. Contrasting to this, the H 2 volume generation was found to decrease continuously over multiple thermochemical cycles using NiFe 2 O 4 nanoparticles as well as NiFe 2 O 4 /Y 2 O 3 powdered mixture of nanoparticles. The transient O 2 profiles were also compared for both the core-shell nanoparticles and powdered mixture during multiple regeneration steps. Detailed transmission electron microscopy (TEM) analysis clearly provided evidence of core-shell morphology with NiFe 2 O 4 core encapsulated by Y 2 O 3 shell. The grain size and morphological properties of as-prepared nanoparticles were compared with the nanoparticles obtained after thermochemical water-splitting reaction using powdered X-ray diffraction, and scanning electron microscopy. V C 2015 AIP Publishing LLC. [http://dx.