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Zirconium-based materials have attracted extended analysis interest because of their high structural practicality, excellent chemical sturdiness, and intractableness. ZrO2 is additionally wide identified to be used as a surrogate for learning the mechanism of UO2 kernel fabrication of High-Temperature Reactor (HTR) fuels. ZrO2 has similar properties to UO2 system in such a way that microbeads are of paramount importance, especially in the case of such nuclear stimuli-responsive systems. This beads stability will be strongly correlated to the precursor composition and the steps of the synthesis process. One of the simple synthesis processes of ZrO2 microbeads is by gelation process, which could be carried out by internal gelation or external gelation. This article will discuss the synthesis result of ZrO2 microbeads system using external gelation process to understand the gelation process with the emphasis will be given to the interaction of PVA-THFA host–ZrO2 guest systems. FTIR and thermal data were thoroughly explored to derive the mechanism during the gelation process concerning conventional gels in describing general aspects of gel formation.