This study aimed to prepare Veitchia merilli coir (VMC) through pre-carbonisation process, followed by chemical activation using potassium hydroxide as an activating agent. The experiment was conducted under different pyrolytic physical activation temperatures of 650, 700, and 750 °C with the code VMS-650, VMS-700, and VMS-750 for each sample. Physical activation methods develop or modify the pore structure, specific surface area, and microstructure of activated carbon. Furthermore, the prepared VMCs were characterised using X-ray diffraction, Fourier transform infrared, scanning electron microscope, energy dispersive X-ray, and cyclic voltammetry with a symmetrical two-electrode system in 1 M H2SO4 solution. The microstructure analysis showed that the VMC carbon electrode has an amorphous structure with two broad peaks at 2θ angles around 26° and 44° corresponding to the (002) and (100) planes, with the L c VMS-700 having a value of 16.007 nm. The VMC electrode has a C≡C carbon bond as a functional group, which extends in bands from 2311.79 to 2373.51 cm−1. Meanwhile, the VMS-700 electrode shows a combined surface morphology of nanofibers as well as mesopores, and the energy dispersive X-ray results showed carbon content of 92.83%. The electrochemical properties of supercapacitor cells indicated this electrode had the highest specific capacitance value of 264.2 F g−1. From the obtained results, the respective physical and electrochemical properties of the carbon electrodes and supercapacitor cells showed that the activated VMC-700 at 700 °C is the optimum temperature to produce the best performance compared to 650 and 750 °C.