Plastic scintillators containing Bi2O3 nanoparticles (NPs) were developed as detectors for X-ray synchrotron radiation. A hydrothermal method was used to synthesize the NPs that had average particle sizes of less than 10 nm. Higher NP concentration led to a higher detection efficiency at 67.4 keV. The light yield of the scintillator containing 5 wt % Bi2O3 NPs was comparable with or higher than that of the commercially available plastic scintillator, EJ 256. The time resolution of the developed scintillation detector equipped with each sample scintillator was approximately 0.6 ns. Dispersion of nanoparticles within plastic scintillators is generally applicable and has wide application as a method for preparation of plastic scintillators for detecting X-ray synchrotron radiation.