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In order to increase the understanding of the thermal degradation mechanism, Fourier transform infrared spectroscopy (FT-IR) and thermogravimetry -mass spectrometric coupling technique (TG-MS) had been used to study the thermal degradation behavior of furan resin used for glassy carbon materials.The curing and carbonization mechanisms of furan resin were mainly investigated; structural changes and volatile products evolved during thermal degradation were analyzed.The results indicate that,during thermal degradation of furan resin added 7wt% phosphorous acid as curing agent, the rupture of C - O bond in the five-membered heterocycle firstly takes place to release oxygen atoms and then does the C - H bond, which enable the molecular chain to cross-link and condense, then lead to the formation of three dimensional networking structure.With the increase of pyrolyzing temperature, the scission of methyl and the opening of furan ring are generated.As a result, the recomposition of molecular chain structure is generated and hexatomic fused ring containing double bonds is built.The main volatile products during thermal degradation of furan resin are H2 O, and a small mount of CO, CO: and CH4.At elevated temperatures, dehydrogenation takes place and H2 is evolved.