Syndiotactic polystyrene pellets were processed into powder form using mechanical (ball milling, rotor milling) and physicochemical (spray drying) techniques with the intention of using it as feed material for selective laser sintering. New materials are an important component in broadening the application window for selective laser sintering but must meet strict requirements to be used. Particles obtained were characterized in size and shape using SEM imaging, analyzed by software, and compared to the product obtained by conventional ball milling. Rotor milling and spray drying proved capable of making spherical powders, yet only rotor milling achieved particles with a mean diameter within the desired range of 45–97 µm. Subsequently, the obtained powders were examined for the effect each processing technique imparts on the intrinsic properties of the material. Differential scanning calorimetry analysis revealed amorphization for all methods and a reduction in crystallinity after processing, however, the reduction in crystallinity was acceptably low for the spray-dried and rotor-milled powders. Ball milling displayed an exceptional reduction in crystallinity, suggesting severe degradation. As a final test, the rotor-milled powder was subjected to single-layer test and displayed good coalescence and smooth morphology, albeit with a large amount of warpage.
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