In Situ Methods for Metal-Flux Synthesis in Inert Environments

Flux growth synthesis is an advantageous synthetic method as it allows for the growth of single crystals of both congruently melting and metastable phases. The determination of synthetic parameters for the flux growth of new crystalline phases is complex as many factors and parameters need to be considered, such as the purity and morphology of the starting material and heating profile variables including maximum temperature, dwell time, cooling rate, and flux removal temperature. In situ monitoring of crystallite growth can lead to elucidation of reaction intermediates and growth mechanisms. The determination of pivotal reaction parameters can revolutionize the way growth parameters are selected. Herein, we report a new sample environment and furnace apparatus for synchrotron in situ synthesis of crystalline materials, including flux grown intermetallics.