Current global population growth has led to higher demands for food production, increasing our reliance on synthetic fertilizers. These are formed via the Haber Process, where nitrogen from air and hydrogen (currently obtained from natural gas combustion) is used to produce the needed ammonia. More sustainable ways of generating hydrogen gas that don’t involve burning fossil fuels are necessary. One possible replacement is nanoscale cobalt phosphide, a known, effective electrocatalyst for the hydrogen evolution reaction (HER), defined as transforming two protons and two electrons into hydrogen gas. However, this electrocatalytic system requires energy input to achieve the transformation. This project investigates the design of a synthesis to produce an indium phosphide/cobalt phosphide (InP/CoP) core/shell structure that can generate H2 photocatalytically. The InP quantum dot will be used to generate a photoexcited electron using visible light, and then this photoexcited electron will be transferred to the CoP catalyst to perform the desired proton reduction step. Regeneration of the quantum dot ground state will be mediated through the use of a sacrificial electron donor. Here we present our findings evaluating several approaches to the colloidal synthesis of the desired core-shell heterostructure using an aminophosphine precursor and the corresponding metal halides. Success of the various syntheses was determined by examining data from multiple characterization techniques including UV-Vis spectroscopy, X-ray diffraction, electron microscopy, and elemental analysis. We expect these methods to be generalizable to a suite of electrocatalytically active transition metal phosphide shell materials. This work will ultimately contribute new methods to the sustainable production of hydrogen for industrial scale applications.