The observation of neutrinoless double beta decay is an important issue in nuclear and particle physics. The development of organic liquid scintillators with high transparency and a high concentration of the target isotope would be very useful for neutrinoless double beta decay experiments. Therefore, we propose a liquid scintillator loaded with metal oxide nanoparticles containing the target isotope. In this work, 6-phenylhexanoic acid-modified ZrO2 nanoparticles, which contain96Zr as the target isotope, were synthesized under sub/supercritical hydrothermal conditions. The effects of the synthesis temperature on the formation and surface modification of the nanoparticles were investigated. Performing the synthesis at 250 and 300◦C resulted in the formation of nanoparticles with smaller particle sizes and higher surface modification densities than those prepared at 350 and 400◦C. The highest modification density (3.1 ± 0.2 molecules/nm2) and Zr concentration of (0.33 ± 0.04 wt.%) were obtained at 300◦C. The surface-modified ZrO2 nanoparticles were dispersed in a toluene-based liquid scintillator. The liquid scintillator was transparent to the scintillation wavelength, and a clear scintillation peak was confirmed by X-rayinduced radioluminescence spectroscopy. In conclusion, 6-phenylhexanoic acid-modified ZrO2 nanoparticles synthesized at 300◦C are suitable for loading in liquid scintillators.