We synthesized plastic scintillators incorporated with HfO2 nanoparticles as detectors for X-ray synchrotron radiation. Nanoparticles with sizes of less than 10 nm were synthesized with the subcritical hydrothermal method. The detection efficiency of high-energy X-ray photons improved by up to 3.3 times because of the addition of the nanoparticles. Nanosecond time resolution was successfully achieved for all the scintillators. These results indicate that this method is applicable for the preparation of plastic scintillators to detect X-ray synchrotron radiation.