ZnSiAs2 (chalcopyrite structure) single crystals were grown by chemical vapor transport (CVT). Hall effect and photoelectrochemical techniques were used to characterize the properties of the p-type materials. Doping level, mobility, and resistivity were determined and compared with literature values for crystals Obtained from other growth techniques; Photocurrent spectroscopy was used to measure the bandgap and transition types in the crystals. The interfacial energetics were measured with capacitance techniques (Mott-Schottky). The effect of various wet chemical etchants on the photocurrent voltage curves and quantum yields for carrier collection was also investigated.