Self-assembled microwires of terephthalic acid (TPA) and melamine are prepared through the evaporation of water in a solution mixture of TPA and melamine. The microwires were characterized by using scanning electron microscope (SEM), attenuated total reflection infrared (ATR-IR) spectra, and cross-polarized optical microscopy (CPOM). The TPA•M microwires showed semi-conductive properties.