Scientific and technological advances over the past four decades have led to an increase in the demand for new technologies as well as improvements in the existing ones. In many cases these improvements involve the development of new materials. In particular, carbon has attached a great deal of interest, since natural carbon materials have extraordinary properties that confer on them a great potential for different applications. However, its impurities and a lack of control over its properties have led to its replacement by synthetic carbonaceous materials. In our research group, we have been working in polymer science since years. A very efficient technique has been developed for the synthesis of one type of polymer named resorcinol-formaldehyde (RF) xerogels, obtained by sol-gel methodology. This synthesis presents many advantages such as a very rapid process (i.e., 4-5 hours versus 4-5 days in a conventional synthesis), a one-pot synthesis, and the possibility of a total control the processes occurring. It is even possible to know which step of the process (heating, polymerization, curing, drying) is occurring, in order to stop the process in a specific step to control the final form of the product. Different aspects of the synthesis process have been studied, such as residence time, temperature or specific power used, and their influence on the final properties of the RF xerogels have been evaluated. Therefore, a completely controlled and efficient process of polymerization is presented for obtaining bespoke materials at a nanoscale