Battery Sample Holders for TTK 600

Importance of the Topic

The study of battery materials under in situ and in operando conditions is critical for understanding structural changes that occur during real‐time charging and discharging. Non‐ambient XRD experiments enable researchers to assess performance under extreme temperatures and varied atmospheres, reflecting realistic operational environments in e‐mobility and grid storage applications.

Objectives and Study Overview

This work presents the first commercial non‐ambient sample holders designed for the Anton Paar TTK 600 stage, allowing coin cell assemblies to be characterized via X‐ray diffraction both in reflection and transmission geometries. The primary objectives were to enable safe sample transfer from glove box to diffractometer, cover a wide temperature range (–180 °C to 130 °C), and maintain mechanical stability for high‐quality diffraction data.

Methodology and Instrumentation

Sample holders feature a gastight compartment into which pre‐assembled coin cells are loaded under an inert atmosphere. A direct heater and dual cooling options (compressed air or liquid nitrogen) deliver rapid temperature ramps. A Pt100 temperature sensor positioned near the sample ensures precise thermal monitoring. Two geometrical configurations (reflection and transmission) accommodate various XRD setups, while window foils are selected based on X‐ray transparency and mechanical robustness.

Main Results and Discussion

Performance tests demonstrated stable operation across the full temperature span with minimal thermal expansion, preserving sample alignment. Fast heating and cooling rates were achieved without compromising positional accuracy. The gastight design successfully maintained inert conditions during transfer and measurement, preventing air‐sensitive battery materials from degradation.

Benefits and Practical Applications

• Direct observation of phase transitions, lattice parameters, crystallite size, and strain under electrical load and temperature stress.
• Enables characterization of battery behavior under realistic extreme‐climate scenarios.
• Compatible with standard laboratory diffractometers for rapid integration.
• High throughput due to easy sample exchange and reliable thermal control.

Future Trends and Potential Applications

Advancements may include integration with electrochemical impedance spectroscopy and synchrotron‐source adaptations for enhanced time resolution. Customizable holders for pouch or cylindrical cells and automation of temperature‐load cycling will further expand analytical capabilities. AI‐driven data analysis could accelerate insights into degradation mechanisms.

Conclusion

The TTK 600 battery sample holders represent a significant step toward routine non‐ambient in operando XRD analysis of coin cells. Their robust thermal management, gastight containment, and flexible geometry support comprehensive study of battery materials under real‐world conditions, advancing both fundamental research and industrial quality control.