Cross-linked polyethylene (XLPE) sheets were thermally deteriorated in atmospheric air at 180°C for at most 100 hours, and microscopic structural changes due to oxidation such as material density, crystallinity, gel fraction and free volumes were evaluated by the Archimedes' technique, the X-ray diffraction method, the gel fraction measurement and the positron annihilation technique, respectively. As a result, it was found that the crystallinity and free volumes decreased after about 40 hours of heating on the upper surface of XLPE sheets where air supply was sufficient during heating and oxidation degree was high. However, on the lower surface that contacted with a metal plate during heating and was less oxidized, changes of crystallinity and free volumes were small after 40 hours of heating. When the crystallinity and free volumes decreased, the material density increased. It was also found that the gel fraction increased at 100 hours of heating. The observation results of cross-sections of XLPE sheets by the transmission electron microscope showed that lamella crystals disappeared after 40 hours of heating especially near the upper surface of XLPE sheets and agree with the change of the crystallinity. Then, the relationships between the material density, the crystallinity and free volumes in the cases of crystalline polymers such as polyethylene without deterioration and XLPE thermally deteriorated at 180°C were discussed.
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