Nano-sized boron carbon oxynitride (BCNO) phosphors around 50nm containing no rare earth metal and free from color heterogeneity were synthesized from mixtures of boric acid, urea, and citric acid by microwave heating with substantially shorter reaction times and lower temperatures than in the conventional BCNO preparation method such as electric-furnace heating. The emission wavelength of the phosphors varied with the mixing ratio of raw materials and it was found that lowering the proportion of urea to boric acid or citric acid tended to increase the internal quantum yield and shorten the emission wavelength under excitation at 365nm. It was also found for the first time that a light-emitting polymer could be synthesized from a mixture of the prepared BCNO nanoparticles and a polyvinyl alcohol. This polymer composite exhibited uniform dispersion and stabilization of the luminescence and had a high internal quantum yield of 54%, which was higher than that of the phosphor alone.