本論文利用光致放光(photoluminescence)、時間解析(time-resolved)、激發(excitation)與紅外線(infrared)光譜研究不同溫度下含水硝酸銪(Eu(NO3)3.5H2O)與硝酸釤(Sm(NO3)3.6H2O)之放光行為。本論文將這兩種化合物由室溫加熱至550°C,分別在不同溫度下(200℃、300℃、400℃、550℃)取其光譜資料,分析其第一激發態與第二激發態之放光行為,發現雖然Eu3+與Sm3+離子大小相近與能階相似,但在加熱過程中其放光性質卻大不相同。含水硝酸釤加熱至400℃過程中放光光譜與衰退曲線變化皆不大,但在400℃以上卻形成不會發光的物種。含水硝酸銪無論是放光光譜或放光衰退曲線,在加熱至200℃以上皆產生明顯變化,推測是加熱過程改變了配位結構,並產生其他物種,如氧化物(Eu2O3)。本論文將以光譜資料闡明此兩種含水硝酸鹽在加熱過程中之結構改變與化學變化。;Photoluminescence (PL), time-resolved, excitation, and infrared (IR) spectra of Eu(NO3)3 ·5H2O and Sm(NO3)3·6H2O were recorded at different temperatures as these two compounds were heated from ambient temperature to 550℃. Spectroscopic data at various temperatures (200℃, 300℃, 400℃, 550℃) were obtained for the analysis of the emission behaviors of their first and second excited states. Despite of the similar size and energy levels between Eu3+ and Sm3+, their emission properties are profoundly different in the heating process. There are only minor changes in the emission spectra and decay curves of Sm(NO3)3·6H2O as heated to 400℃, but some non-radiative species are formed above 400℃. In contrast, there are dramatic changes in the emission spectra and decay curves in heating Eu(NO3) 3·5H2O above 200℃. These changes could come from the change of coordination environments and the formation of other species such as Eu2O3. This thesis will elucidate the structural and chemical changes of these two water-containing nitrates in the heating process.