將熱蒸鍍法製作出五組不同粒徑的鉛奈米粉粒，進行X光繞射分析，得知鉛奈米粉粒隨時間改變的繞射譜圖，可明顯看出氧化反應造成繞射譜圖的改變。為了更深入了解鉛奈米粉粒的氧化機制，利用Rietveld結構精算法，來分析X光繞射實驗所得的譜圖，進而獲得精細的晶體結構與參數。由結構精算法的結果，我們了解氧化過程所造成結構上的改變，Pb及其氧化物結構排列的相似之處，重量百分比隨時間變化的情形，Pb原子與O原子間相互的關係等，進而推論鉛奈米粉粒的氧化機制。 We fabricated the Pb nanoparticlesin five different diameters by thermal evaporation method,and proceeded the X-ray diffraction experiment. We could get the X-ray diffraction illustrations of Pb nanoparticleswith the passes of time, and obtain the change of diffraction illustrations which caused by oxide reation. In order to understand the oxidative mechanics of Pb nanoparticles, we used GSAS to analyze the X-ray diffraction illustrations, and then obtained the fine crystal structures and parameters. According to the results, we could understand the changes in structure which caused by the process of oxidation, the similar crystal structure between Pb and its oxide, the situation of percentage changes with time, and the relation between Pb and O. Then we could assume that the oxidative mechanics of Pb nanoparticles.