School of Mechanical and Aerospace Engineering, Queens University Belfast, Belfast, UK.
J Mater Sci Mater Med. 2010 Aug;21(8):2307-16. doi: 10.1007/s10856-009-3963-2. Epub 2009 Dec 23.
Ibuprofen loaded poly(epsilon-caprolactone) (PCL) layered silicate nanocomposites were prepared by hot-melt extrusion. The morphology and extent of dispersion of ibuprofen and layered silicate was studied using a combination of wide-angle X-ray diffraction (WAXD), field emission scanning electron microscopy (FESEM) and high resolution transmission electron microscopy (HRTEM). Exhaustive examination across the length scales revealed the composite to have both an intercalated and exfoliated morphology. The ibuprofen was well dispersed and distributed throughout the PCL matrix. Most significantly, the static tensile and dynamic mechanical properties of PCL can be manipulated as a function of nanoclay loading and is dependent on the aspect ratio of clay platelets. The glass transition of PCL increased by up to 16 degrees C on addition of nanoclay, as determined from dynamic mechanical thermal analysis (DMTA). This behaviour was attributed to the constrained mobility of PCL chains intercalated between clay platelets and to the tethering of PCL chains by hydrogen bonding with platelet edges. As a consequence, PCL crystallisation was inhibited and confirmed from non-isothermal crystallisation experiments using differential scanning calorimetry (DSC). The fraction of PCL that was crystalline (X(c)) decreased by 15% on addition of ibuprofen and nanoclay, although the temperature of crystallisation (T(c)) did not change significantly. The dissolution of ibuprofen from PCL can be retarded by addition of layered silicates (nanoclays) to the polymer matrix.
布洛芬负载聚己内酯(PCL)层状硅酸盐纳米复合材料通过热熔挤出法制备。采用广角 X 射线衍射(WAXD)、场发射扫描电子显微镜(FESEM)和高分辨率透射电子显微镜(HRTEM)相结合的方法研究了布洛芬和层状硅酸盐的形态和分散程度。跨尺度的详细检查表明,该复合材料具有插层和剥离的形态。布洛芬在 PCL 基体中得到了很好的分散和分布。最重要的是,PCL 的静态拉伸和动态力学性能可以作为纳米粘土负载的函数进行操纵,并且取决于粘土片层的纵横比。从动态力学热分析(DMTA)可以看出,添加纳米粘土后,PCL 的玻璃化转变温度提高了 16°C。这种行为归因于插层在粘土片层之间的 PCL 链的受限迁移以及 PCL 链与片层边缘的氢键的束缚。因此,PCL 的结晶受到抑制,并通过使用差示扫描量热法(DSC)进行的非等温结晶实验得到证实。尽管结晶温度(T(c))没有显著变化,但添加布洛芬和纳米粘土后,PCL 的结晶分数(X(c))降低了 15%。通过向聚合物基质中添加层状硅酸盐(纳米粘土)可以延缓布洛芬从 PCL 中的溶解。