Rapid phase elucidation of polycrystalline materials is essential for developing new materials of chemical, pharmaceutical and industrial interest. Yet, the size and quantity of many crystalline phases are too small for routine X-ray diffraction analysis. This has become a workflow bottleneck in materials development, especially in high-throughput synthesis screening. Here we demonstrate the application of serial rotation electron diffraction (SerialRED) for high-throughput phase identification of complex polycrystalline zeolite products. The products were prepared from a combination of multiple framework T atoms ([Si,Ge,Al] or [Si,Ge,B]) and a simple organic structure-directing agent. We show that using SerialRED, five zeolite phases can be identified from a highly complex mixture. This includes phases with ultra-low contents undetectable using X-ray diffraction and phases with identical crystal morphology and similar unit cell parameters. By automatically and rapidly examining hundreds of crystals, SerialRED enables high-throughput phase analysis and allows the exploration of complex synthesis systems. It provides new opportunities for rapid development of polycrystalline materials.

多晶材料的快速相澄清对于开发具有化学、制药和工业意义的新材料至关重要。然而，许多晶相的尺寸和数量对于常规 X 射线衍射分析来说太小。这已成为材料开发中的工作流程瓶颈，特别是在高通量合成筛选中。在这里，我们演示了串行旋转电子衍射 (SerialRED) 在复杂多晶沸石产品高通量物相识别中的应用。该产品由多个骨架T原子（[Si,Ge,Al]或[Si,Ge,B]）和简单的有机结构导向剂的组合制备。我们证明，使用 SerialRED，可以从高度复杂的混合物中识别出五种沸石相。这包括使用 X 射线衍射无法检测到的超低含量相以及具有相同晶体形态和相似晶胞参数的相。通过自动快速检查数百个晶体，SerialRED 可实现高通量相分析并允许探索复杂的合成系统。为多晶材料的快速发展提供了新的机遇。