Two kinds of SiOC(H) particles having intrinsic photoluminescence (PL) spectra were prepared from silicone resin microspheres by heat treatment in a hydrogen atmosphere at 800 or 1100°C. The obtained particles were painted on a Si substrate using a binder, and ion-beam-luminescence spectra were observed under proton beam irradiation with an acceleration energy in the range of 13 MeV. Observed spectra had peaks at wavelength of 520540 nm. These peak wavelengths were larger than those observed under UV light irradiation. The luminescence of H 2 1100 (sample decarbonized at 1100°C) was bright, and that of H 2 800 (sample decarbonized at 800°C) was faint. However, the intensity of luminescence decreased rapidly at an early stage of the beam irradiation. In air, a sharp luminescence band with a peak at 300 nm appeared together with the main emission with a peak in the range of 520540 nm. The existence of the sharp band at 300 nm was apparent in the H 2 800 spectra, whereas it appeared as a minor peak in the H 2 1100 spectra in air.