Porous carbon felts (CFs) are widely used electrode materials for vanadium redox flow batteries (VRFBs). These materials differ in their precursor material, thickness, or graphitization degree and demonstrate broad differences in electrochemical performance. Prior to operation, an activation step, such as acid or heat treatment (HT), is commonly performed to improve their performance. A thermal treatment in air functionalizes the surface of the electrode and improves reaction kinetics as well as the wettability of the electrode. Herein, pristine and heat‐treated CFs are compared regarding their electrolyte wetting behavior for the use in VRFB. Contact angle (CA) measurements are conducted ex situ to investigate the effect of the HT. Furthermore, the porous CFs are examined in situ with an in‐house‐built flow cell regarding their invasion behavior with different types of electrolytes by X‐ray radiography. Additionally, the distribution of the electrolyte inside the felts is investigated by X‐ray tomography. The results demonstrate the effect of the HT and choice of electrolyte on the wetting behavior and electrolyte distribution.
