This thesis investigates the structural and surface-property changes of resorcinol–formaldehyde (RF) carbon aerogels after incorporating graphene oxide (GO). Using NMR cryoporometry and NMR relaxometry, the work reveals how GO affects pore-size distribution, wettability, and liquid–solid interactions. The results show that GO-modified aerogels exhibit more hydrophilic surfaces and more uniform pore accessibility compared to unmodified aerogels. Cryoporometry data confirmed shifts in melting/freezing behavior, while relaxometry demonstrated changes in T₂ distributions linked to altered pore dynamics. Overall, the study provides clear evidence that even small amounts of GO significantly influence both the physical structure and fluid-interaction behavior of carbon aerogels.