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Automated laboratory x-ray diffractometer and fluorescence spectrometer for high-throughput materials
Hyun Sang Park1, Timothy Long1, Michael Wall1
1Johns Hopkins University, Baltimore, Maryland 21218, USA.
The Review of Scientific Instruments
|June 24, 2026
Summary
A new automated instrument enables simultaneous X-ray diffraction and fluorescence spectroscopy for rapid materials characterization. This high-throughput system accelerates data generation for artificial intelligence and machine learning in materials research.
Area of Science:
- Materials Science
- Analytical Chemistry
- Instrumentation
Background:
- Growing demand for automated, high-throughput characterization in materials research.
- Need for rapid large dataset generation for AI and machine learning applications.
- Limitations of existing techniques in speed and automation.
Purpose of the Study:
- Introduce and evaluate a novel instrument for simultaneous X-ray diffraction (XRD) and X-ray fluorescence (XRF) spectroscopy.
- Optimize the instrument for high-throughput studies of combinatorial specimens.
- Demonstrate the instrument's capability in rapid dataset creation for materials research.
Main Methods:
- Development of a new instrument integrating XRD and XRF spectroscopy.
- Utilized a bright, focused, high-energy X-ray beam (24 keV) and a pixel array area detector for spatially resolved transmission diffraction.
- Employed a silicon drift detector for spatially resolved elemental composition analysis via XRF.
- Implemented fully automated specimen handling and data orchestration for autonomous processing.
Main Results:
- Achieved spatially resolved (∼200 μm) diffraction measurements on thick specimens (>100 μm) with short exposure times (as low as 1 s).
- Enabled simultaneous, spatially resolved elemental composition measurement using XRF.
- Demonstrated high-throughput data generation through automated sample manipulation and data processing.
- Successfully applied the instrument to a combinatorial study of Cu-Ti alloys.
Conclusions:
- The developed instrument significantly enhances throughput for materials characterization.
- Automated XRD and XRF spectroscopy facilitates rapid data acquisition for AI-driven materials discovery.
- The system provides a powerful tool for combinatorial materials studies and large dataset generation.
