The sensing characteristics of toluene gas are monitored by fabricating ZnO nanorod structures. ZnO nanostructured sensor materials are produced on a Zn film via an ultrasonic process in a 0.01 M aqueous solution of C6H12N4 and Zn(NO3)2∙6H2O. The response of the sensors subjected to heat treatment in oxygen and nitrogen atmospheres is improved by 20% and 10%, respectively. The improvement is considered to be correlated with the increase in grain size. The relationship between the heat treatment and sensing characteristics is evaluated.