Small-angle X-ray scattering (SAXS) is used to characterize the in situ formation of diblock copolymer spheres, worms and vesicles during reversible addition–fragmentation chain transfer (RAFT) aqueous dispersion polymerization of 2-hydroxypropyl methacrylate at 70 °C using a poly(glycerol monomethacrylate) steric stabilizer. ¹H NMR spectroscopy indicates more than 99% HPMA conversion within 80 min, while transmission electron microscopy and dynamic light scattering studies are consistent with the final morphology being pure vesicles. Analysis of time-resolved SAXS patterns for this prototypical polymerization-induced self-assembly (PISA) formulation enables the evolution in copolymer morphology, particle diameter, mean aggregation number, solvent volume fraction, surface density of copolymer chains and their mean inter-chain separation distance at the nanoparticle surface to be monitored. Furthermore, the change in vesicle diameter and membrane thickness during the final stages of polymerization supports an ‘inward growth’ mechanism.

中文翻译：

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典型RAFT水性分散聚合配方的原位SAXS研究：监测聚合诱导的自组装过程中共聚物形态的演变

小角X射线散射（SAXS）用于表征在70°C下使用甲基丙烯酸2-羟丙酯的可逆加成-断裂链转移（RAFT）水性分散聚合过程中二嵌段共聚物球体，蠕虫和囊泡的原位形成。聚（单甲基丙烯酸甘油酯）空间稳定剂。^1个1 H NMR光谱表明在80分钟内HPMA的转化率超过99％，而透射电子显微镜和动态光散射研究与最终形态为纯囊泡一致。分析这种典型的聚合诱导的自组装（PISA）制剂的时间分辨SAXS模式，可以实现共聚物形态，粒径，平均聚集数，溶剂体积分数，共聚物链的表面密度及其平均链间分离的演变要监测的纳米颗粒表面的距离。此外，在聚合反应的最后阶段，囊泡直径和膜厚度的变化支持“向内生长”机制。