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Scandium is a rare earth element that has been declared a critical raw material by the EU. Its availability is low but the demand for it is increasing. Bauxite residue presents a possible European source. A novel process to extract scandium from the residue incorporates anti-solvent crystallization, which delivers the scandium salt (NH4)3ScF6 that can be calcined to ScF3 for direct use in an aluminum alloy. However, this crystallization process produces small crystals in the single-digit micrometer scale, hindering solid–liquid separation. In order to facilitate the separation, the crystallization process needs to be better understood and controlled. Therefore, nucleation kinetics are investigated by measuring the metastable zone width (MSZW) with an optical endoscope probe inside a 300 mL stirred fed-batch crystallizer with varying operating parameters. To study the influence of mixing on the MSZW, the stirring rate, the antisolvent addition rate, and the dilution of the antisolvent before injection are varied. The latter is proven to widen the MSZW by a multiple. It could be confirmed that mixing times on different scales greatly influence the MSZW and the growth of the crystals in the process. With these results, the boundaries for operating parameters are studied in order to control the crystallization process and thus crystal growth.