In this contribution, we report the synthesis and characterization of NixFe3-xO4 and CoxFe3-xO4 redox nanomaterials using sol-gel method. These materials will be used to produce solar fuels such as H2 or syngas from H2O and/or CO2 via solar thermochemical cycles (STCs). For the sol-gel synthesis of ferrites, the Ni, Co, Fe precursor salts were dissolved in ethanol and propylene oxide (PO) was added dropwise to the well mixed solution as a gelation agent to achieve gel formation. Freshly synthesized gels were aged, dried, and calcined by heating them to 600°C in air. The calcined powders were characterized by powder x-ray diffractometer (XRD), BET surface area, as well as scanning (SEM) and transmission (TEM) electron microscopy. Their suitability to be used in STCs for the production of solar fuels was assessed by performing several reduction/re-oxidation cycles using a thermogravimetric analyzer (TGA).