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In this work, a thermally reduced graphene oxide (TRGO) thin film on microscopic glass was prepared using spray coating and atmospheric pressure chemical vapour deposition. The structure of TRGO was analysed using X-ray diffraction (XRD) spectroscopy, scanning electron microscope (SEM), energy-dispersive X-ray spectroscopy (EDS), Fourier transform infrared (FTIR) spectroscopy, and ultraviolet–visible spectroscopy (UV-Vis) suggesting a decrease in oxygen functional groups (OFGs), leading to the restacking, change in colour, and transparency of the graphene sheets. Raman spectrum deconvolution detailed the film’s parameters, such as the crystallite size, degree of defect, degree of amorphousness, and type of defect. The electrochemical performance of the microsupercapacitor (µ-SC) showed a rectangular cyclic voltammetry shape, which was maintained at a high scan rate, revealing phenomenal electric double-layer capacitor (EDLC) behaviour. The power law and Trasatti’s analysis indicated that low-temperature TRGO µ-SC is dominated by diffusion-controlled behaviour, while higher temperature TRGO µ-SC is dominated by surface-controlled behaviour.