利用小角/广角X射线散射联用及一维相关函数分析研究聚(ε-己内酯)片晶的形态  

STUDY OF LAMELLAR MORPHOLOGY OF POLY (ε-CAPROLACTONE) BASED ON SAXS/WAXS SIMULTANEOUS MEASUREMENT AND ONE-DIMENSIONAL CORRELATION FUNCTION ANALYSIS

作　　者：于翔[1] 陈尔强[2] 朱诚身[1] 何素琴[1] 刘文涛[1] 

机构地区：[1]郑州大学材料科学与工程学院,郑州450052 [2]北京分子科学国家实验室高分子化学与物理教育部重点实验室北京大学化学与分子工程学院,北京100871

出　　处：《高分子学报》2010年第9期1136-1142,共7页Acta Polymerica Sinica

基　　金：国家自然科学基金(基金号20774006);北京大学"研究生访学项目"资助

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(ε-己内酯) 片晶 广角X射线散射 小角X射线散射 一维相关函数 

分 类 号：O633.14[理学—高分子化学]