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The utilization of a zirconium oxide (ZrO2) thin film as the insulator in a metal–insulator–semiconductor (MIS) capacitor to enhance the characteristics of thin‐film transistors is investigated. Although the high crystallinity of ZrO2 is favorable to achieving higher capacitance density in metal–insulator–metal capacitors with ZrO2 thin films, it decreases the capacitance with increasing applied bias in Mo/ZrO2/InGaZnO (IGZO)‐structured MIS capacitors. Through comprehensive physical, chemical, and electrical characterizations, this study investigated the mechanism underlying the decreasing capacitance with increasing the applied bias in the accumulation state of the Mo/ZrO2/IGZO‐structured MIS capacitor depending on the crystallinity of ZrO2. Furthermore, the investigation identifies the optimal crystal structure of ZrO2 thin films for IGZO‐based MIS capacitors, highlighting the importance of forming meso‐crystalline structures in high dielectric constant (k) materials to enhance the k value and mitigating the decrease in capacitance caused by the accumulated carrier loss through grain boundaries of ZrO2. [ABSTRACT FROM AUTHOR]