Grade 91 steel (modified 9Cr-1Mo steel) is considered a prospective material for the Next Generation Nuclear Power Plant for application in reactor pressure vessels at temperatures of up to 650 °C. In this study, heat treatment of Grade 91 steel was performed by normalizing and tempering the steel at various temperatures for different periods of time. Optical microscopy, scanning and transmission electron microscopy in conjunction with microhardness profiles and calorimetric plots were used to understand the microstructural evolution including precipitate structures and were correlated with mechanical behavior of the steel. Thermo-Calc™ calculations were used to support the experimental work. Furthermore, carbon isopleth and temperature dependencies of the volume fraction of different precipitates were constructed.