Understanding polymer nanostructures is a prerequisite to manipulate their physical properties. Molecular self-assembly under confinement effectively generates novel polymer nanostructures. However, in one confined system, diffraction signals of different nanostructures are merged in a typical two-dimensional (2D) wide-angle X-ray diffraction (WAXD) measurement. For comparison, selected-area electron diffraction (SAED) of transmission electron microscopy can precisely capture the “local” diffraction signal of an individual nanoscale entity. Here, using isotactic polypropylene (i-PP) as a model polymer, we have demonstrated a cross-analysis of global X-ray and local electron diffraction results to fully reveal the structural details of i-PP nanorods. For the first time, we have decomposed completely the “mixed” 2D WAXD patterns of i-PP nanorods into five types of α-phase nanostructures: (a). Left-tilted daughter crystals; (b) Right-tilted daughter crystals; (c) Double-tilted daughter crystals; (d) a*-axis oriented crystals; (e) b-axis oriented crystals.

了解聚合物纳米结构是操纵其物理性质的先决条件。限制条件下的分子自组装有效地产生了新颖的聚合物纳米结构。但是，在一个封闭的系统中，不同的纳米结构的衍射信号会在典型的二维（2D）广角X射线衍射（WAXD）测量中合并。为了进行比较，透射电子显微镜的选择区域电子衍射（SAED）可以精确捕获单个纳米级实体的“局部”衍射信号。在这里，使用全同立构聚丙烯（i-PP）作为模型聚合物，我们证明了对X射线和局部电子衍射结果的交叉分析，以充分揭示i-PP纳米棒的结构细节。首次，我们已将i-PP纳米棒的“混合”二维WAXD模式完全分解为五种类型的α相纳米结构：（a）。左倾斜子晶体；（b）右倾子晶体；（c）双倾斜子晶体；（d）a *轴取向的晶体；（e）b轴取向的晶体。