In investigations of carbon-based materials, non-destructive Raman spectroscopy is a primary diagnostic tool owing to the broad range of information it can provide to monitor the composition of such materials. It is useful especially for determining the presence of point defects and in semi-quantitatively measuring annealing defects or the presence of contaminants [1-5]. In addition to spectral analysis by Raman spectroscopy, confocal Raman mapping will also be used to directly visualize the local distribution of microelectrode constituents and the presence and location of unwanted defects or residues. Since the structural properties of the candidate microelectrodes are essential for achieving the proposed research, detailed characterizations will be performed at The University of Texas at El Paso (UTEP). Aim - Assessment of microelectrodes structural homogeneity through spectroscopic and microscopic analysis. Structural changes associated with the distribution of different constituents (i.e., sp3 or sp2 hybridized carbon) throughout the doped diamond thin film and the extent of defects will be analyzed in detail using spectroscopic and microscopic confocal Raman. The functionalization of the substrate surface, which can be of carbon fiber or diamond, and the extent of dopant permeation will be examined, too. The results of this research will serve as reference points for further investigations of the microelectrodes to in vitro and in vivo FSCV, MCSWV, and fixed-potential amperometry measurements. The latter analysis will be performed at the Mayo Clinic.