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In situ wide-angle X-ray scattering together with infrared imaging was performed during three-dimensional material extrusion printing and correlated with the development of the crystalline structure and subsequent thermomechanical properties. Identical samples were printed with nozzle motion either along the short axis or the long axis. The short axis mode had higher thermal retention, which resulted in later onset of crystal structure. The longer time spent at temperatures between the glass transition and the melting point produced samples with higher degree of crystallinity but also significantly increased brittleness. The tracer diffusion coefficient D(T), together with its temperature dependence, was measured using neutron reflectivity, and the total interdiffusion length between filaments was then calculated using D(T) for each temperature point, as determined by the measured thermal profiles. This allowed us to …