By using a fuel cell having a membrane electrode assembly having and electrolyte membrane 100 formed by a polymer electrolyte membrane, and an anode 101 and a cathode 102 carrying a catalytic metal and sandwiching electrolyte membrane 100. The anode 101 and the cathode 102 are in electrical connection, and an activation treatment is carried out for opening an active site of catalytic metal of the cathode 102. This provides an activation method of a polymer electrolyte fuel cell which is advantageous to activation and raises cell voltage.