Inert matrix (IM) materials for nuclear fuel in light water reactors must meet several critical requirements that include high temperature stability, good irradiation behaviour, high thermal conductivity, and hot water corrosion resistance. MgO possesses all of the necessary requirements for an ideal IM candidate, except hot water corrosion resistance. A composite approach is being investigated in order to improve the corrosion resistance of MgO, while simultaneously taking advantage of the high thermal conductivity of MgO and its ability to be reprocessed in nitric acid. MgO–pyrochlore composite compositions are fabricated based on neutronic property simulations for assessment as potential IM materials. The selected pyrochlore compositions are synthesized by both sol gel and solid state processing, and how composite processing affects the microstructure will be discussed. Among the multiple composite processing approaches investigated, ball milling produces the most homogeneous and consistent microstructures.