A novel electrode for an NO gas sensor was fabricated from electrospun polyacrylonitrile fibers by thermal treatment to obtain carbon fibers followed by chemical activation to enhance the activity of gas adsorption sites. The activation process improved the porous structure, increasing the specific surface area and allowing for efficient gas adsorption. The gas sensing ability and response time were improved by the increased surface area and micropore fraction. High performance gas sensing was then demonstrated by following a proposed mechanism based on the activation effects. Initially, the pore structure developed by activation significantly increased the amount of adsorbed gas, as shown by the high sensitivity of the gas sensor. Additionally, the increased micropore fraction enabled a rapid sensor response time due to improve the adsorption speed. Overall, the sensitivity for NO gas was improved approximately six-fold, and the response time was reduced by approximately 83% due to the effects of chemical activation. Keywords : Gas sensor, Electrospun fiber, Pore structure, Sensitivity, Response time