In this study, ZnO-SnO2 heterojunction nanofibers were fabricated using electrospinning and treated by Ar plasma. The post treatment demonstrated the ability to regulate adsorbed oxygen of nanofibers and thus affecting the gas sensing performance. The results revealed that the gas sensing performances increased with the increase of plasma treatment time at first, then showed a downward trend. The setting for the best H-2 gas performance was 20 min of plasma treatment, under which the response of the sample was 80% higher and the response time was two thirds shorter than those of the untreated sample. The explanation can be that appropriate plasma treatment can increase the oxygen vacancy on the surface of heterojunction nanofibers as well as the resistance modulation range in the air; however, excessive plasma treatment can result in the reduction of the resistance modulation range in the air by reducing the metal oxide to metal.