Successful anodic deposition of ethynyl terminal 1,4diethynylbenzene on carbon fiber microelectrodes has been demonstrated for the first time. Single scan deposition of DEB resulted in a smooth film layer on the CFM surface that resulted in similar characteristics as that of an unmodified electrode, including adsorption coefficient to Cu(II) and net impedance across perturbation frequencies in EIS. One-scan DEB coated electrodes also had similar sensitivity towards Cu(II) in an FSCV measurement as that of an unmodified electrode. Three-scan deposition of DEB resulted in island-like structures on the CFM surface, a rough surface that prevented monolayer coverage by Cu(II), and a three-fold higher sensitivity towards Cu(II) compared to the bare CFM. This elevated sensitivity persisted even in the presence of other divalent interfering species (Zn(II), Mg(II), Ca(II)) and for up to four days when stored at room temperature. Characterization experiments revealed that 3scan DEB modified electrodes had reduced double layer capacitance and increased nonideal capacitor behavior compared to bare electrodes.