The rate at which the world’s population is expanding is concerning, as it has led to a rise in the need for fossil fuels, resource depletion, and environmental harm. The fast exhaustion of fossil fuel reserves has posed a significant obstacle to fulfilling forthcoming energy requirements. Because fossil fuels are scarce and global greenhouse gas levels are growing, we need to lessen our heavy reliance on them. These factors compelled nations all around the world to look for new fuel sources. Much attention has been paid to the use of biofuels as a possible substitute for lessening the adverse impacts of an excessive reliance on fossil fuels. There is still work to be done to enhance the output, quality, and sustainability of biofuels, despite significant efforts to boost the commercial realization of biofuel production. Environmentally friendly renewable biofuels may now be produced and improved with the help of nanotechnology, which has proven to be a unique and efficient method. Because of their high reactivity and high surface-to-volume ratio, nanomaterials are more efficient in the processing and manufacturing of biofuel. With an emphasis on the synthesis of biofuels, this chapter has mostly explored the green synthesis of various nanomaterials and the techniques for characterizing them.