A high-temperature furnace for multimodal synchrotron-based X-ray microscopy and diffraction imaging

Area of Science:

• Materials Science
• Experimental Physics
• Synchrotron Radiation

Background:

• In situ synchrotron X-ray experiments require specialized sample environments capable of controlled high-temperature manipulation.
• Existing furnace designs may limit sample accessibility or compatibility with advanced X-ray techniques.

Purpose of the Study:

• To design, calibrate, and demonstrate the application of a novel non-contact high-temperature furnace for synchrotron X-ray experiments.
• To achieve stable operation up to 1000°C with precise temperature control and high heating rates.
• To ensure compatibility with various X-ray diffraction and imaging techniques.

Main Methods:

• Development of a 3D-printed modular non-contact furnace with 360° rotation and tilt capabilities.
• Temperature calibration using thermocouples for ramp rates and gradient mapping.
• Synchrotron X-ray diffraction to monitor phase transitions (ferrite to austenite) under beamline conditions.
• Implementation at the European Synchrotron Radiation Facility (ESRF) ID03 beamline.

Main Results:

• Stable operation up to 1000°C achieved, with heating rates >6000°C/min and thermal stability ±2°C.
• Full sample accessibility and compatibility with techniques like dark-field X-ray microscopy (DFXM).
• Demonstrated application on an Al1050 sample showing strain relaxation and grain growth during isothermal annealing via DFXM.

Conclusions:

• The developed non-contact furnace is a robust, flexible, and customizable platform for high-temperature in situ synchrotron studies.
• It facilitates advanced materials characterization across diverse fields, including metals, ceramics, and energy materials.
• The furnace is available to users at the ESRF, promoting further research in materials science.