New methods for synthesis of active materials have been developed to improve capacity and cycle life performance of lithium-ion batteries. Past studies have focused on routes of development of materials and new processes, which might not be economical for large-scale production. In this regard, this study examines a widely employed carbothermal reduction technology for the synthesis of lithium-iron phosphate (LiFePO4/C) and investigates effects of process conditions during this synthesis on final battery performance. An experimental combined genetic programming approach is used to model the effects of crucial process conditions (sintering time, the carbon content, and the sintering temperature) on the discharge capacity of the assembled battery. Experiments are conducted to collect the discharge capacity data based on varying LiFePO4/C synthesis conditions, and genetic programming is employed to develop a suitable functional relationship between them. The results show that the battery discharge capacity is controlled significantly by adjusting sintering temperature and carbon content, while the effect of sintering time is found to be insignificant. Further, the interaction effect of the sintering time and carbon content is much more obvious than that of the sintering time and the sintering temperature. The findings from the study pave the way for the optimum design of the synthesis process of LiFePO4/C for a higher battery performance.