While continuously alarming reports regarding climate disasters appear in the media, the need for reduction of CO₂ emissions becomes more urgent. An interesting solution is converting the harmful CO₂ into a value-added chemical, such as methanol. The CO₂ reduction can be realized in a photoelectrochemical cell, using a combination of solar energy and renewable electricity to provide the necessary energy. To design this system, efficient and selective semiconducting photoelectrodes which are also stable, low cost and non-toxic are needed.^1,2 To achieve this, key characteristics of the photoelectrodes include for example their conduction band edge and bandgap. The aim in this project is to fabricate the CuFeO₂ delafossite as a photocathode material. The delafossite is attractive as a natural p-type semiconductor that, compared to cuprous oxide, has shown a higher electrochemical stability, improved hole mobility and less susceptibility to photodegradation. However, it is challenging to synthesize this material, as it is a metastable, high temperature phase, existing only between 1015°C and 1090°C according to the thermodynamic copper-iron oxide phase diagram.³ Therefore, in the research at hand, a hydrothermal synthesis route for the delafossite CuFeO₂ was studied. In general, hydrothermal methods are good candidates for the synthesis of metastable phases at low temperature. However, in literature, the hydrothermal synthesis for CuFeO₂ is often reported without much attention to the detailed effects of the many different synthesis parameters nor to controlling reproducibility, which is known to require great care. Therefore, a systematic investigation of the synthesis process was conducted by a variation of important synthesis parameters such as the Cu/Fe ratio, reaction time and temperature. It was concluded that the formation of the delafossite CuFeO₂ was obtained via a solution-based hydrothermal process after 12 hours at 120°C at various Fe/Cu ratios except for the Fe/Cu 1/1 ratio. The phase formation was verified by x-ray diffraction and Raman spectroscopy. Furthermore, the bandgap was studied with UV-vis spectroscopy and the sample surface and morphology were studied with TEM and Raman mapping. In conclusion, the CuFeO₂ delafossite appears to have the potential to be a promising photocathode material for CO₂ reduction.