Microscopic proton conductivity at surfaces of a hydrocarbon-type polymer electrolyte membrane of sulfonated poly(arylene ketone) block copolymers (SPK-bl-1) was investigated by current-sensing atomic force microscopy (CS-AFM) under a hydrogen atmosphere. The distributions of proton-conductive regions on the SPK-bl-1 membrane surfaces were different on two surface sides of the membrane: the substrate side and the air side after being cast on a poly(ethylene terephthalate) substrate. After a liquid-water treatment of the membrane at 60 degrees C, the surface morphology of both sides changed. The proton-conductive area and the "pseudo current density" increased especially on the substrate side, and the difference between two sides of the membrane became very small. The scanning transmission electron microscopy inside the membrane showed no structural change after the hot-water treatment, and the water uptake and conductivity of the membrane were also unchanged. This hot liquid-water treatment activating the membrane surfaces should be related to the conditioning processes of the membrane-electrode assemblies of polymer electrolyte fuel cells. (C) 2014 Elsevier Ltd. All rights reserved.