In Situ 4D STEM of LiNiO2 Particles Heated in an Oxygen Atmosphere: Toward Investigation of Solid-State Batteries Under Realistic Processing Conditions

Atmosphere AX Publication Alert in Small Methods for Battery Studies

Tuesday Publication Post! 📖 Understanding how cathode active materials (CAMs) evolve during high-temperature processing is critical for advancing next-generation solid-state batteries. Using the #AtmosphereAX, this study from Thomas Demuth, Shamail Ahmed, Philipp Kurzhals, Johannes Haust, Jürgen Belz, Andreas Beyer, Jürgen Janek, and Kerstin Volz establishes an in situ heating methodology capable of probing battery materials in an oxygen atmosphere with the spatial precision of (S)TEM.

Using LiNiO₂ (LNO) as a model CAM, the researchers tracked its morphological and structural evolution during high-temperature treatment via in situ 4D-STEM, supported by postmortem diffraction and spectroscopy. The results revealed:

🔥 Onset of structural degradation at ~350 °C, where LNO transitions from its layered R̄3m phase to a NiO-type rock-salt structure
☁️ A markedly higher degradation temperature in oxygen compared to vacuum-based in situ heating
🔋 Clear evidence that realistic atmospheric conditions are essential for accurately assessing material stability

These insights highlight the importance of oxygen-environment TEM for understanding interfacial reactions, degradation pathways, and processing limits in solid-state battery materials. This capability paves the way for more reliable, more durable energy storage technologies.

Want to read the entire work? Find it here!
https://www.doi,org/10.1002/smtd.202500357

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