Structure of grain boundaries in wet, synthetic polycrystalline, statically recrystallizing halite - evidence from cryo-SEM observations

It is well known from nature and experiments that the presence of brine strongly affects the microstructural evolution and the mechanical and transport properties of halite. Existing interpretations of the grain boundary structure in deformed, wet, salt samples annealed statically at room temperature are based on indirect evidence from reflected light microscopy and conventional scanning electron microscopy. This paper presents direct observations of fluid-filled grain boundaries using the cryogenic-scanning electron microscope (cryo-SEM) in which the grain boundary fluids were frozen before breaking the samples. The rapid cooling transforms the brine into two phases, i.e. ice and hydrohalite, which are easily recognized from characteristic segregation patterns. We studied samples of wet, synthetic, polycrystalline halite annealed under static conditions at room temperature. In coarse-grained samples, fine-scale segregation patterns were observed at the boundaries of the primary recrystallizing grains. These points indicate the existence of fluid films with a thickness in the range of 30 nm, but the finer scale structure of the fluid remains unknown. In fine-grained samples, the distribution and reorganization of fluids with annealing time is recorded by the combination of contact healing and successive accumulation of fluids in triple junction tubes. The contact healing is attributed to the small initial grain size, such that the fluid film necks down by accumulating the fluids into previously existing triple junctions via neck growth. Electron backscatter diffraction measurements of both primary and secondary recrystallized grains indicate that they are euhedral, i.e. the grain growth morphology is controlled by the anisotropy of the grain boundary energy of the growing grain, which results in planar growth faces.