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

TL;DR

This paper presents a versatile, high-temperature furnace designed for in situ synchrotron X-ray experiments, enabling detailed imaging and diffraction studies of materials up to 1000°C with high stability and flexibility.

Contribution

The authors introduce a customizable, non-contact furnace compatible with multiple synchrotron techniques, featuring rapid heating, precise temperature calibration, and full translational and rotational freedom.

Findings

Successfully calibrated temperature using thermocouple and diffraction methods

Demonstrated imaging of grain evolution during annealing

Furnace supports diverse materials science experiments

Abstract

The design, calibration, and initial application of a non-contact high-temperature furnace developed for in situ synchrotron X-ray experiments are presented. The system enables a stable operation up to 1000 {\deg}C, with heating rates exceeding 6000 {\deg}C/min and thermal stability better than {\pm}2 {\deg}C. Temperature calibration was performed using (i) direct measurements with a thermocouple to characterize heating and cooling ramp rates and map temperature gradients along the x, y, and z axes, and (ii) synchrotron X-ray diffraction to track the ferrite-to-austenite (BCC to FCC) phase transition in an iron grain under beamline conditions. The furnace's contactless geometry provides full translational and rotational freedom, with 360{\deg} rotation and wide tilt capabilities, making it fully compatible with a range of diffraction and imaging techniques. Its 3D-printed modular body includes closable apertures for auxiliary functions such as active cooling or X-ray fluorescence. The design is easily customizable for diverse experimental requirements and can be adapted to most beamlines. The furnace has been implemented at the ID03 beamline of the European Synchrotron Radiation Facility (ESRF) which supports Dark field X-ray Microscopy (DFXM), 3D X-ray Diffraction (3DXRD), magnified topotomography (MTT), phase-contrast tomography (PCT) and diffraction contrast tomography (DCT). As a first application, a DFXM case study on a cold-rolled Al1050 sample during isothermal annealing is presented. The imaging of a selected grain before and after the heat treatment reveals strain relaxation and grain growth. This furnace offers a robust and flexible platform for high-temperature synchrotron studies across materials science, including metals, ceramics, and energy materials. It is now part of the ESRF sample environment pool and is available to all users.