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This work presents an application of Raman spectroscopy as a tool to investigate heterogeneity in the composition of carbon materials obtained electrochemically. A combination of Raman maps and histograms has been used to describe samples synthesized via wet chemistry. The results showed that a simple evaluation of an average spectrum or one single spectrum per sample would have hidden important compositional variations present in the film. The Raman maps revealed heterogeneous hydrogenation in different areas of the carbon films, whereas histograms described the statistical relevance of the classification of the different types of carbon materials. The effect of electrosynthesis parameters on the quality of the films was also investigated. As the deposition time increased, the carbon films showed higher homogeneity in their spatial composition. The nature of the electrolyte led to differences in film functionalization and on the degree of hydrogenation.

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An economical and facile method to synthesize a precursor for carbon films and materials has been developed. This precursor can be easily coated onto substrates without binder reagents and then converted into a graphitic-like structure after mild thermal treatment. This approach potentially allows the coating of glass surfaces of different shapes and forms, such as the inside of a glass tube, for instance. The precursor consists of tetrahedral halocarbyne units which randomly combine through single electron transfer with organometallic compounds to create a poly(carbyne)-like polymeric material. Advanced characterization tools reveal that the synthesized product (poly(halocarbyne) or PXC, where X indicate the presence of halogens, is composed mostly of carbon, hydrogen, and a variable percentage of residual halocarbon groups. Therefore, it possesses good solubility in organic solvents and can be coated on any complex substrate. The coated PXC material produced here was annealed under mild conditions, leading to the production of a graphitic-like film on a glass substrate. The chemical homogeneity of the carbon material of the film was confirmed by Raman spectroscopy.