In this work, carbon nanofibers(CNFs) were prepared by using electrospinning method. Phosphoric acid and sodium carbonate activation of CNFs were conducted to increase surface area and pore volume. Pore structures of activated CNFs were developed with increasing surface area and pore volume through activation. Specific surface area increased about 60 times and total pore volume developed around 120 times. Activated CNFs have different pore distribution with different chemical agent.