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Sol‐gel and hand milling techniques were used to prepare a lithium iron phosphate‐lithium manganese silicate (LiFePO4−Li2MnSiO4) hybrid cathode materials. The structural studies from x‐ray diffraction (XRD) and high resolution transmission electron microscopy (HRTEM) show that the materials are well crystallized although few impurities were observed in the pristine LiFePO4 (LFP) and Li2MnSiO4 (LMS) materials. We used graphene to coat the hybrid cathode materials in order to increase its conductivity and enhance the electrochemical performance. The successful reduction of the graphene oxide into graphene nanosheets was confirmed with the results from the Fourier transform infrared (FTIR) and Raman spectroscopy. The morphological analysis indicate that the pristine materials are made of spherical nanoparticles that are slightly agglomerated while the sol‐gel‐prepared hybrid cathode materials show evenly distributed spherical nanoparticles with minimal agglomeration. The in situ sol‐gel technique gave more homogenously mixed material in comparison to the hand milling method and particle sizes of 37 and 23 nm respectively were obtained for the plain, and graphenised sol gel derived hybrid materials. The sol‐gel derived hybrid materials are also the most thermally stable giving a total weight loss of 4.5 % and 3.4 % for the plain and graphenised cathodes respectively. While the LFP‐LMS hybrid cathode materials performed better electrochemically more than the pristine materials in terms of enhanced current and specific capacities, the graphenised LFP‐LMS hybrid cathode materials showed better electrochemical properties compared to those without graphene. This is associated with the presence of graphene nanosheets in these samples. All the results confirmed that the graphenised LiFePO4−Li2MnSiO4 hybrid cathode material prepared via in situ sol‐gel method performed better than those of the hand milling method. [ABSTRACT FROM AUTHOR]