Powder X-ray diffraction (PXRD) is a key technique for the structural characterisation of solid-state materials, but compared with tasks such as liquid handling, its end-to-end automation is highly challenging. This is because coupling PXRD experiments with crystallisation comprises multiple solid handling steps that include sample recovery, sample preparation by grinding, sample mounting and, finally, collection of X-ray diffraction data. Each of these steps has individual technical challenges from an automation perspective, and hence no commercial instrument exists that can grow crystals, process them into a powder, mount them in a diffractometer, and collect PXRD data in an autonomous, closed-loop way. Here we present an automated robotic workflow to carry out autonomous PXRD experiments. The PXRD data collected for polymorphs of small organic compounds is comparable to that collected under the same conditions manually. Beyond accelerating PXRD experiments, this workflow involves 13 component steps and integrates three different types of robots, each from a separate supplier, illustrating the power of flexible, modular automation in complex, multitask laboratories.

翻译：粉末X射线衍射（PXRD）是固态材料结构表征的关键技术，但与液体处理等任务相比，其端到端自动化极具挑战性。这是因为将PXRD实验与结晶过程耦合涉及多个固体处理步骤，包括样品回收、研磨制样、样品装样以及最终的X射线衍射数据采集。从自动化角度看，每个步骤均存在独立的技术难题，因此目前尚无商业仪器能够以自主闭环方式完成晶体生长、粉末化处理、衍射仪装样及PXRD数据采集。本文提出了一种自动化机器人工作流程，用于执行自主PXRD实验。针对小分子有机化合物多晶型采集的PXRD数据，与在相同条件下人工采集的数据质量相当。该工作流程不仅加速了PXRD实验，还包含13个组件步骤，并集成了来自三家不同供应商的三种类型机器人，展示了灵活模块化自动化的能力在复杂、多任务实验场景中的强大优势。