In this investigation, the aqueous corrosion resistance of 9Cr series heat-resistant steel during tempering was investigated. Optical Microscopy (OM), Scanning Electron Microscopy (SEM), and Energy Dispersive Spectrometer (EDS) were used to analyze the effect of tempering temperature on the microstructure and precipitation behavior of precipitates. The heat-resisting steel was heated to 1150 °C for 1 h, and then tempered at different temperatures between 680 °C and 760 °C for 2 h. The microstructure of the heat-resistant steel after tempering was composed of lath-tempered martensite and fine precipitates. The hardness decreased with increasing tempering temperature, ranging from HBW 261 to HBW 193. The aqueous corrosion resistance improved as the tempering temperatures increased from 680 °C to 720 °C but deteriorated at higher temperatures, such as 760 °C, which was obtained by an electrochemical corrosion performance test. The aqueous corrosion resistance was affected by the decrease in dislocation density and the decrease in Cr solution in the tempered martensite. With the increase in the tempering temperature, the aqueous corrosion potential first increases and then decreases, the self-corrosion current density first decreases and then increases, and the polarization resistance first increases and then decreases. Furthermore, the increase in corrosion resistance is attributed to the reduction in dislocation density and chromium depletion in the martensitic structure as the tempering temperature approaches 720 °C. This paper reveals the effect of tempering temperature on the corrosion resistance of 9Cr series heat-resistant steel, which is a further exploration of a known phenomenon.