Zhang Daohai, He Min, He Weidi, Zhou Ying, Qin Shuhao, Yu Jie
Department of Polymer Material and Engineering, College of Materials and Metallurgy, Guizhou University, Guiyang 550025, China.
National Engineering Research Center for Compounding and Modification of Polymeric Materials, Guiyang 550014, China.
Materials (Basel). 2017 May 4;10(5):500. doi: 10.3390/ma10050500.
In this work, the long glass fibre-reinforced poly(butylene terephthalate) (PBT) composites filled with 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) were prepared by melt blending, and the influence of thermo-oxidative ageing on the static and dynamic mechanical properties, thermal behaviours and morphology of composites with different ageing time at 120 °C were investigated and analysed. The results showed that the mechanical properties decreased in the primary stage of ageing, while embrittlement occurs in the later period, and the crystallinity of PBT decreases first, and then recovers to some extent. The scanning electron microscopy (SEM) photos of the samples indicated that the obvious crack appeared on the sample surface and a deeper, broader crack occurred with a longer ageing time. The results of energy dispersive X-ray analysis (EDAX) proved the DOPO filler diffused to the sample surface by measuring the content of phosphorus. Thermal gravimetric analysis (TGA) curves showed that the thermal stabilities of composites increased with longer ageing time, as did the values of the limited oxygen index (LOI). Meanwhile, the results of dynamic mechanical analysis (DMA) indicated that the glass transition temperature shifted to a higher temperature after ageing due to the effect of crosslinking, and both the crosslinking and degradation of PBT molecular chains act as the main factors in the whole process of thermo-oxidative ageing.
在本工作中,通过熔融共混制备了填充9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)的长玻璃纤维增强聚对苯二甲酸丁二醇酯(PBT)复合材料,并研究和分析了热氧化老化对120℃下不同老化时间复合材料的静态和动态力学性能、热行为及形态的影响。结果表明,在老化初期力学性能下降,后期出现脆化,PBT的结晶度先降低,然后有所恢复。样品的扫描电子显微镜(SEM)照片表明,样品表面出现明显裂纹,且随着老化时间延长,裂纹更深、更宽。能量色散X射线分析(EDAX)结果通过测量磷含量证明了DOPO填料扩散到样品表面。热重分析(TGA)曲线表明,复合材料的热稳定性随着老化时间延长而提高,极限氧指数(LOI)值也如此。同时,动态力学分析(DMA)结果表明,由于交联作用,老化后玻璃化转变温度向更高温度移动,PBT分子链的交联和降解在热氧化老化全过程中均起主要作用。