Design of a robot-automated flat plate/reflection geometry x-ray diffraction setup for accelerated materials discovery and structural screening.

Abstract

We report the design, construction, and automation of a flat plate sample loading, alignment, and data acquisition system for x-ray diffraction measurements in reflection geometry implemented at the Stanford Synchrotron Radiation Lightsource. The system is built onto a single platform, enabling facile transferability, and is compartmentalized into sample storage, sample transfer, and sample position/alignment segments. The core feature of this system is a six-axis robotic arm that offers a large range of highly reproducible and programmable movements. The degrees of freedom of the robot arm enable adaptability in which movements can be modified to fit various beamline environments and sample configurations. The samples are housed on 3D printed sample mounts, which are arranged onto a 6 × 2 array of sample cassettes capable of holding seven samples. Using sample mounts designed for solid oxide electrolysis button cells (SOECs), the maximum tray capacity is 84 samples, which can be aligned and run in ∼24 h with long exposure scans. The sample array is additionally capable of accommodating a range of sample sizes and geometries due to the rapid 3D printed fabrication. The components of the setup will be described in detail and performance will be demonstrated with a set of representative SOEC and XRD standard samples. Opportunities for future developments and integration with the automated setup are summarized.