A study has been performed to assess the possibilities of fique fibers (a Colombian native fiber) as reinforcement for polymeric matrices. The fique fibers were treated using different chemical surface treatments. The effects produced on the physico-mechanical properties of fique fibers have been investigated. The applied surface treatments have been mercerization, and/or chemical agents such as maleic anhydride and acrylic acid, and also silanization. In order to analyze the chemical changes in the treated fibers, Fourier Transform Infrared, FTIR, spectroscopy was used along with two related techniques: Attenuated Total Reflection (ATR) and Coupled Microscopy. Additionally, physical and mechanical properties of untreated and treated fique fibers have been studied. A wettability study using contact angle measurements has also been performed for surface free energy determination. The thermal stability of the fibers has been investigated by thermogravimetrycal analysis.