In-Situ Heating X-Ray Diffraction of LiNi0.6Mn0.3Co0.1O2 and LiNi0.7Mn0.3O2 Made Using the All-Dry Synthesis Process
Date
2025-06
Authors
Yu, Svena
Bond, Toby
Rahemtulla, Al
Leontowich, Adam
Thompson, Daphne
Dahn, J. R.
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Wiley
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Article
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Abstract
In-situ synthesis X-ray diffraction is conducted at the Canadian Light Source to probe phase changes during the all-dry synthesis of LiNi0.6Mn0.3Co0.1O2 (NMC631) and LiNi0.7Mn0.3O2 (NM73) made using either LiOH·H2O or Li2CO3. All materials are heated up to 950 °C and held for one hour at 950 °C under flowing oxygen. The pathway to a layered phase is similar for all samples. First, a lithiated manganese oxide phase is formed at low temperature, then cations are incorporated into a rock salt phase from ≈420 °C. A spinel intermediary phase is formed before cation ordering occurs between Li and transition metal ions above 800 °C, giving rise to the intended layered hexagonal structure. Amongst the three materials tested, the layered phase of NMC631 (made using LiOH·H2O) evolves at the lowest temperature of ≈820 °C and refines rapidly during the high temperature hold. The melting of LiOH coincides nicely with the oxidation of Ni, which forms the basis for the rock salt structure. It is postulated that the molten LiOH facilitates cation diffusion into the rock salt phase, allowing for an earlier formation of the layered phase in comparison to using Li2CO3, which has a higher decomposition temperature.
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all-dry synthesis, LiOH NMC631, low temperature
Citation
Yu, S., Bond, T., Rahemtulla, A., Leontowich, A. F. G., Thompson, D., & Dahn, J. R. (2025). In-Situ Heating X-Ray Diffraction of LiNi0.6Mn0.3Co0.1O2 and LiNi0.7Mn0.3O2 Made Using the All-Dry Synthesis Process. Small Methods, e2500632-. https://doi.org/10.1002/smtd.202500632
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DOI
https://doi.org/10.1002/smtd.202500632