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

Journal Article · · Review of Scientific Instruments
DOI: https://doi.org/10.1063/5.0198335 · OSTI ID:2513870
 [1];  [2];  [2];  [3];  [3];  [2]
  1. SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States). Stanford Synchrotron Radiation Lightsource (SSRL); SLAC National Accelerator Laboratory
  2. SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States). Stanford Synchrotron Radiation Lightsource (SSRL)
  3. National Renewable Energy Laboratory (NREL), Golden, CO (United States)

Here, 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 programable 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. Samples are housed on 3D printed sample mounts, which are arranged onto a 6 × 2 array of sample cassettes capable of holding 7 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 hours 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.

Research Organization:
National Renewable Energy Laboratory (NREL), Golden, CO (United States); SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States)
Sponsoring Organization:
USDOE Office of Energy Efficiency and Renewable Energy (EERE), Office of Sustainable Transportation. Hydrogen Fuel Cell Technologies Office (HFTO); USDOE Office of Science (SC), Basic Energy Sciences (BES)
Grant/Contract Number:
AC02-76SF00515; AC36-08GO28308
OSTI ID:
2513870
Report Number(s):
NREL/JA--5900-93634
Journal Information:
Review of Scientific Instruments, Journal Name: Review of Scientific Instruments Journal Issue: 2 Vol. 96; ISSN 0034-6748
Publisher:
American Institute of Physics (AIP)Copyright Statement
Country of Publication:
United States
Language:
English

References (13)

Adaptively driven X-ray diffraction guided by machine learning for autonomous phase identification journal March 2023
Array programming with NumPy journal September 2020
SciPy 1.0: fundamental algorithms for scientific computing in Python journal February 2020
High-throughput screening with micro-x-ray fluorescence journal June 2005
High-throughput x-ray characterization system for combinatorial materials studies journal September 2005
High energy x-ray diffraction/x-ray fluorescence spectroscopy for high-throughput analysis of composition spread thin films journal December 2009
Automated laboratory based X-ray beamline with multi-capillary sample chamber journal August 2013
Autonomous micro-focus angle-resolved photoemission spectroscopy journal May 2024
Remote access to crystallography beamlines at SSRL: novel tools for training, education and collaboration journal August 2010
Mail-in data collection at SPring-8 protein crystallography beamlines journal April 2008
A six-axis robotic sample changer for high-throughput neutron powder diffraction and texture measurements journal November 2014
Remote and automated high-throughput powder diffraction measurements enabled by a robotic sample changer at SSRL beamline 2-1 journal September 2023
Robotic sample changers for macromolecular X-ray crystallography and biological small-angle X-ray scattering at the National Synchrotron Light Source II journal August 2021

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