We have preliminarily developed the part of experimental study about UF4 materials and its thermal chemical reaction characteristics in air, respectively with deferent analysis techniques such as micro-laser Raman spectroscopy(MLRS), X-ray photoelectron spectroscopy(XPS), weighing up and observing metallographs etc. Based on the physical and chemical properties of UF4 , we have obtained the Raman and XPS spectra of different uranium compounds after heating in stated temperature and time . The experimental results indicated that , UF4 sample is equivalent stable until it has been heated to 200 ℃ in air , and its Raman spectra was almost no change . But heated above 250 ℃ in air , the surface color of UF4 sample has obviously been changed , and there have been formed into multiform uranium compounds such as UO2、UO2F2、U3O8 etc with Raman and XPS analysis . On the other hand, the chemical reaction rate of UF4 in air was showed the trend from fast to slow.