Natural fibers have become a valuable resource in the composite industry; however, their use is limited due to their low compatibility with traditional polymeric matrices. That low compatibility promotes low mechanical strength in the composite material. In order to avoid this, it is necessary to treat the reinforcement material or the matrix before the composite manufacturing. This paper presents the results of a research aimed to study the effect of two compatibilization techniques applied to natural fibers, on the mechanical properties of the composite. The analyzed techniques were sodium hydroxide (NaOH) baths acting as coupling agent, as well as treatments using a dry etching plasma (physical sputtering). Natural fibers employed in this research were obtained from Guadua angustifolia bamboo culms, and the manufacturing of the composite was accomplished using a manual moulding technique and a polyester matrix. Results revealed that treatments using sodium hydroxide decrease the fibers' tensile strength, while the dry etching plasma treatments do not appear to affect their tensile strength. Moreover, both compatibilization techniques improve guaduapolyester composites' strength. It is believed that this increment is the result of the increase in the bonding strength between composite's phases.