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In this paper, the PMMA films doped with N,N'-diphenyl-N,N'-di(m-tolyl)-benzidineand rubrene were fabricated by spin coating, and the effect of photooxidation onthe photoluminescence of the doped PMMA thin films was investigated. The resultsshowed that under the irradiation of 350nm UV light, N,N'-diphenyl-N,N'-di(m-tolyl)-benzidine can sensitized rubrene and results in the enhancement in the photooxrationof rubrene. The effect of photooxidation on the photoluminescence from rubrene w asmore obvious. Both lifetime measurement and in situ measurement of photolumines-cence showed that rubrene molecules exist in two chemical surroundings.