The novel nitride-based luminescent materials have received much attention since the end of the last century. In this paper, the commercial Eu2＋-activated nitride red phosphors, Sr1.95Si5N8：Eu0.05, Sr1.85Si5N8：Eu0.15 and Ca0.99AlSiN3：Eu0.01 phosphors were an-nealed at different temperatures （beyond 300 oC） to investigate the dependence of their luminescence performance and structure vari-ability on the temperature. By photoluminescence spectra, X-ray diffraction （XRD） and thermogravimetry-differential scanning calo-rimetry （TG-DSC） analysis, the high temperature stability of the hosts and activator of the three samples were disclosed. With the an-nealing temperature increasing, the activator Eu2＋ions were firstly oxidized and then host in Sr1.95Si5N8：Eu0.05 and Sr1.85Si5N8：Eu0.15, but for Ca0.99AlSiN3：Eu0.01, only the oxidation of the host could be observed, which would lead to the luminescence degradation and even failure of these phosphors. The activator Eu2＋ions were much more stable in CaAlSiN3：Eu than Sr2Si5N8：Eu due to their crystal surroundings, and its concentration also influenced the temperature stability of Sr2Si5N8：Eu.
