作　　者： ; ; ; ; ;

机构地区： 郑州大学材料科学与工程学院

出　　处： 《高分子学报》 2010年第9期1136-1142,共7页

摘　　要： 用小角/广角X射线散射(SAXS/WAXS)联用的实验方法考察了等温结晶温度(Tc)和等温时间对聚(ε-己内酯)(PCL)片晶形态的影响.根据WAXS数据计算了PCL的重量结晶度,进而求得其体积结晶度Vc(WAXS).在不同Tc下结晶的PCL样品的Vc(WAXS)均略高于50%.对SAXS谱线做一维相关函数(1DCF)分析,得到了PCL的片晶长周期(LP)和无定形层厚度(La).通过比较WAXS及SAXS的数据分析结果,认为PCL晶体需用"三相模型"予以描述,其过渡层厚度(E)约为LP的15%～18%,对片晶形态具有重要影响.随着Tc升高,PCL晶体的Lc、La及E均逐渐增大,但Lc的变化率最大,这使得结晶度上升.在50℃等温结晶不同时间,发现Lc随延长时间显著增加,而La及E则不断减小.等温10天后,PCL晶体的SAXS谱线上可观察到5级散射,表明片晶相当完善. The effects of isothermal crystallization temperature（Tc） and crystallization time on the lamellar morphology of poly（ε-caprolactone） were investigated by using simultaneous measurement of wide-angle/small-angle X-ray scattering（SAXS/WAXS） and one-dimensional correlation function（1DCF） analysis.On the basis of the weight fraction of crystallinity obtained from WAXS result,we calculated the volume fraction crystallinity [Vc（WAXS）]of PCL,which was slightly larger than 50%.The 1DCF analysis of SAXS profiles gave the long period（LP） and thickness of the amorphous region（La）.Comparing the data deduced from the WAXS and SAXS experimental result,we considered that the＂three-phase＂model is preferable to the＂twophase＂model for the PCL crystal.The calculated thickness of the transition zone between the crystalline and amorphous region（E） was of 15% ～ 18% of the LP,showing great influence to the lamellar morphology.With increasing Tc,the values of Lc increased faster than that of La and E,leading to the increase of crystallinity.During isothermal crystallization at 50℃,the Lc of PCL was increased with increasing isothermal time,whereas the La and E were decreased accordingly.After isothermal crystallization at 50℃ for 10 days,the PCL sample with Vc（WAXS） of 61% gave a SAXS profile with the multiple scattering peaks up to the fifth order,indicating that the lamellar structure was rather perfect.

关 键 词： 聚 己内酯 片晶 广角 射线散射 小角 射线散射 一维相关函数

领　　域： [理学] [理学]