New millimeter-wave thermal analysis instrumentation has been developed and studied for characterization of materials required for diverse fuel and structural needs in high temperature reactor environments such as the Next Generation Nuclear Plant (NGNP). A two-receiver 137 GHz system with orthogonal polarizations for anisotropic resolution of material properties has been implemented at MIT. The system was tested with graphite and silicon carbide specimens at temperatures up to 1300 ºC inside an electric furnace. The analytic and hardware basis for active millimeter-wave radiometry of reactor materials at high temperature has been established. Real-time, non contact measurement sensitivity to anisotropic surface emissivity and submillimeter surface displacement was demonstrated. The 137 GHz emissivity of reactor grade graphite (NBG17) from SGL Group was found to be low, ~ 5 %, in the 500-1200 °C range and increases by a factor of 2 to 4 with small linear grooves simulating fracturing. The low graphite emissivity would make millimeter-wave active radiometry a sensitive diagnostic of graphite changes due to environmentally induced stress fracturing, swelling, or corrosion. The silicon carbide tested from Ortek, Inc. was found to have a much higher emissivity at 137 GHz of ~90% Thin coatings of silicon carbide on reactor grade graphite supplied by SGL Group were found to be mostly transparent to millimeter-waves, increasing the 137 GHz emissivity of the coated reactor grade graphite to about ~14% at 1250 ºC.