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Carbon fibers (CFs) decorated by Co 2 P nanoparticles and carbon nanotubes were prepared via needle-less electrospinning technique. Formation of catalytically active Co 2 P nanoparticles and growth of carbon nanotubes were monitored in open and closed sintering environment at different sintering exposure times. Higher porosity, important in the catalytic reaction for easier penetration of electrolyte into the CFs, was achieved by mixing two immiscible polymers with natrium dodecyl sulfate and subsequent heat treatment process. Structure and morphology of the prepared modified carbon fibers were characterized by XRD, SEM and TEM. The time of heat exposure at the sintering temperature of 1200 °C and closure of the sintering space showed distinct effect on the growth and shape of carbon nanotubes. SEM and Raman spectroscopy revealed that closure of the system led to the formation of carbon nanotubes with smaller diameters and less structural disorder. Comparing of as-prepared CFs revealed that CFs with Co 2 P sintered in the closed system exhibited the best electrocatalytic activity for hydrogen evolution reaction due to lower overpotential and smaller Tafel slope in acidic solution.