ADVANCED MATERIALS & PROCESSES | OCTOBER 2025 31 (the intensity ratio of the D band to the G band) for both corroded graphite and graphene. This shift unequivocally signals an accumulation of defect density attributable to oxidative damage. Furthermore, the G band, indicative of the sp2 hybridized carbon network, exhibited a noticeable frequency shift, correlating with strain induction within the material’s lattice due to environmental stressors. For graphene, the 2D band, highly sensitive to the number of layers, displayed reduced intensity and broadening, highlighting the loss of monolayer characteristics and the onset of interlayer stacking during prolonged degradation. Conversely, samples subjected to protective surface coatings or dopants exhibited significantly lower ID/IG ratios and minimal shifts in their G and 2D bands, providing compelling evidence of effective structural preservation. Infrared Spectroscopy. IR spectro- scopy offered a detailed chemical fingerprint of the functional groups formed during material oxidation. For graphite, distinct absorption bands characteristic of hydroxyl (-OH) and carbonyl (C=O) groups were clearly discernible in the IR spectra. The emergence of these surface oxidation products directly correlated with observed reductions in the material’s electronic conductivity and an increase in its mechanical brittleness. Post- treatment IR analysis confirmed that polymer coatings effectively mitigated the formation of these deleterious functional groups, thereby substantially improving graphene’s stability in aggressive corrosive environments. capable of both characterizing degradation mechanisms in situ and informing mitigation strategies. This article delineates the transformative impact of advanced spectroscopy as a foundational toolkit for deciphering the molecular-level intricacies of carbon-based materials. Raman spectroscopy, for instance, provides exquisite sensitivity to phonon confinement effects, enabling the precise identification of structural defects and polymorphic transformations. Com- plementarily, IR spectroscopy yields detailed insights into specific functional groups and surface passivation layers, while XPS offers quantitative elemental composition and oxidation state analysis, critical for understanding surface reactivity and interfacial phenomena. Through the judicious application of these techniques, researchers can systematically fine-tune material per- formance, extend device operational lifetimes, and devise innovative solutions for pervasive issues such as corrosion in fuel cells and industrial coatings. The study rigorously demonstrates the substantial contribution of these spectroscopic techniques to a deeper understanding of carbon materials across diverse applications— from high-performance batteries and efficient fuel cells to resilient corrosion protection. This work highlights the synergistic imperative between cutting- edge materials science and advanced analytical methodologies in forging efficient and sustainable energy systems. METHODOLOGY The investigation employed a dual approach, integrating experimental procedures with a comprehensive literature review to elucidate the properties and performance of carbon materials. Initial sample preparation involved synthesizing graphite and graphene using established methods such as chemical vapor deposition (CVD) and mechanical exfoliation, ensuring high purity and consistent quality for reliable characterization. To simulate operational degradation, samples were subjected to various corrosive environments, including acidic, alkaline, and saline solutions, mirroring the stresses encountered by electro- chemical energy devices during their service life. KEY TECHNIQUES FOR SPECTROSCOPIC CHARACTERIZATION Raman spectroscopy was employed to assess structural integrity, defect density, and overall material quality. This involved meticulous analysis of the D, G, and 2D bands, which provide characteristic fingerprints of carbon’s structural order and disorder. IR facilitated the detection of specific functional groups formed during oxidative processes, serving as direct indicators of surface chemical transformations. XPS provided quantitative information on surface elemental composition and oxidation states, crucial for understanding surface reactivity and passivation mechanisms. Beyond spectroscopic methods, electrochemical techniques were utilized to evaluate the electrochemical stability of carbon materials. Cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) were particularly informative, characterizing material behavior under varying electrical conditions. Finally, multivariate statistical techniques were applied to establish correlations between spectroscopic data, electrochemical performance, and observed corrosion rates. This comprehensive analysis not only enabled the precise identification of material degradation but also illuminated the influence of factors such as interlayer stacking in multilayer graphene on these degradation processes. RESULTS: SPECTROSCOPIC INSIGHTS INTO CORROSION MECHANISMS Raman Spectroscopy. Raman spectroscopy proved instrumental in resolving subtle structural alterations in carbon materials exposed to corrosive environments. A significant observation was the increase in the ID/IG ratio HORIBA LabRAM Soleil Raman Confocal Imaging Microscope.
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