Corn wet distillers' fiber (corn fiber) is a byproduct of the corn-ethanol production process, with high potential as a precursor for activated carbon due to its moderate nitrogen content and availability. However, there has been limited investigation into activated carbons from the corn fiber. In this work, we produce activated carbons from the corn fiber using three procedures, including direct KOH activation, hydrothermal carbonization (HTC) followed by KOH activation, and FeCl3-catalyzed HTC followed by KOH activation. Catalytic HTC with FeCl3 was found to slightly increase the degree of carbonization relative to uncatalyzed HTC while also removing the nitrogen content at increasing concentrations and slightly increasing the porosity. The resulting activated carbon samples are then characterized by thermal gravimetric analysis, Fourier transform infrared spectroscopy, scanning electron microscopy, and nitrogen analysis. The two-step process resulted in activated carbon with substantially higher surface areas than the one-step process (1220 vs 789 m2/g), as well as much higher thermal stability and nitrogen content (up to 1.20%). The results show that the corn fiber has potential for activated carbon production, with the two-step HTC followed by the activation process producing more favorable material properties than direct activation.