In fuel cells both the anode and cathode electrocatalysts are generally composed of nanosized metal particles which are supported on high surface area materials. The electrochemically active surface area (EASA), of catalysts used in low temperature fuel cells, such as polymer electrolyte membrane fuel cells (PEMFC, fed with hydrogen), direct alcohol fuel cells (DAFCs, alcohols: ethanol, methanol, polyalcohols), and direct formic acid fuel cells (DFAFC), has been found to be greatly enhanced when high surface area carbon-based materials are used as the support. As described in detail in Chap. 3, at the anode of a PEMFC dihydrogen is oxidized yielding protons and electrons. The protons pass through the cation exchange membrane toward the cathode where they are used in the reduction of oxygen to water together with the electrons arriving from the anode. The use of an anionexchange polymeric membrane as electrolyte, i.e., a membrane which allows only negative charges to pass, favors the production of negative ions, in this case OH -, in the process of oxygen reduction at the cathode, while the overall electrochemical process is left unvaried, as well as the reversible voltage of the cell. In PEMFCs, the polymeric electrolyte is generally Nafion Ò , a proton-exchange fluorinated membrane, about 50-200 lm thick. This withholds negatively charged ions (usually sulfonate groups -SO 3 -) covalently bonded to the polymeric backbone and therefore allows the passage of protons. Electrons are therefore forced to flow through the outer circuit. Nafion Ò , like other proton-exchange polymeric membranes, is most efficient when it works between 70 and 100°C, thus limiting the functionality of PEMFCs to low temperature operation.In DAFCs at the anode alcohols are oxidized to yield protons, electrons, and CO 2 or carboxylates, depending on the nature of the alcohol used as a fuel, while the cathode process is wholly similar to the one that takes place in PEMFCs.The most important component of a fuel cell is the membrane electrode assembly (MEA) that is composed of a catalytic layer where the electrochemical reactions occur, a diffusion layer providing access to the fuel and oxygen to the catalytic layer and a membrane where ions flow from one electrode to the other.