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A way to obtain graphene-based materials on a large-scale level is by means of chemical methods for the oxidation of graphite to obtain graphene oxide (GO), in combination with thermal, laser, chemical and electrochemical reduction methods to produce reduced graphene oxide (rGO). Among these methods, thermal and laser-based reduction processes are attractive, due to their fast and low-cost characteristics. In this study, first a modified Hummer’s method was applied to obtain graphite oxide (GrO)/graphene oxide. Subsequently, an electrical furnace, a fusion instrument, a tubular reactor, a heating plate, and a microwave oven were used for the thermal reduction, and UV and CO2 lasers were used for the photothermal and/or photochemical reduction. The chemical and structural characterizations of the fabricated rGO samples were performed by Brunauer–Emmett–Teller (BET), X-ray diffraction (XRD), scanning electron microscope (SEM) and Raman spectroscopy measurements. The analysis and comparison of the results revealed that the strongest feature of the thermal reduction methods is the production of high specific surface area, fundamental for volumetric energy applications such as hydrogen storage, whereas in the case of the laser reduction methods, a highly localized reduction is achieved, ideal for microsupercapacitors in flexible electronics.

Laser-induced graphene (LIG) is a graphenic material synthesized from a polymeric substrate through point-by-point laser pyrolysis. It is a fast and cost-effective technique, and it is ideal for flexible electronics and energy storage devices, such as supercapacitors. However, the miniaturization of the thicknesses of the devices, which is important for these applications, has still not been fully explored. Therefore, this work presents an optimized set of laser conditions to fabricate high-quality LIG microsupercapacitors (MSC) from 60 µm thick polyimide substrates. This is achieved by correlating their structural morphology, material quality, and electrochemical performance. The fabricated devices show a high capacitance of 22.2 mF/cm2 at 0.05 mA/cm2, as well as energy and power densities comparable to those of similar devices that are hybridized with pseudocapacitive elements. The performed structural characterization confirms that the LIG material is composed of high-quality multilayer graphene nanoflakes with good structural continuity and an optimal porosity.