ACF/ZnO photocatalyst was synthesized by a sol-gel method using activated carbon fiber (ACF) and Zn $(NO_3)_2$ as precursors. Samples were characterized by Brunauer-Emmett-Teller measurements (BET), scanning electron microscope (SEM), X-ray diffraction (XRD), and energy dispersive X-ray (EDX). The XRD results showed that ACF/ZnO composites only included a hexagonal phase by heat-treated temperature at $400^{circ}C$, $500^{circ}C$, $600^{circ}C$, and $700^{circ}C$. The SEM analysis revealed that the ACF/ZnO composites did not exhibit any morphological changes of the catalyst surface according to the different heat-treated temperatures. The photocatalytic activity of the samples was tested for degradation of methylene blue (MB) solutions under ultraviolet (UV) light and ultrasonication respectively. The results showed that the photocatalytic activity of ACF/ZnO composites heat-treated at $500^{circ}C$ was higher than other samples, which is ascribed to the fine distribution of ZnO particles on the surface of the ACF. In addition, an ultrasound of low power (50 W) was used as an irradiation source to successfully induce ACF/ZnO composites to perform sonocatalytic degradation of MB. Results indicated that the sonocatalytic method in the presence of ACF/ZnO composites is an advisable choice for the treatments of organic dyes.