ABSTRACTSmall-angle neutron scattering (SANS) is increasingly used to obtain statistically-representative data on particle or pore sizes, number and volume fractions, morphology and total surface areas in technological materials. Until recently, however, it had not been possible to perform in-situ microstructural investigations during thermal treatment. This paper reports on a new high-temperature (up to 1700°C) SANS furnace for materials research. Two interchangeable inner furnaces were built for a single outer atmosphere chamber so that either an oxidizing, a reducing, or a neutral environment can be used. Results derived during sintering of a controlled-porosity silica gel will be presented. The new furnace has made it possible for the first time to measure total porous surface areas and the evolution of pore sizes in situ during densification without interruption. Such measurements are expected to lead to improved process models offering quantitative predictability of product microstructures from the processing history of real materials.