In-Situ Heating X-Ray Diffraction of LiNi0.6Mn0.3Co0.1O2 and LiNi0.7Mn0.3O2 Made Using the All-Dry Synthesis Process
| dc.contributor.author | Yu, Svena | |
| dc.contributor.author | Bond, Toby | |
| dc.contributor.author | Rahemtulla, Al | |
| dc.contributor.author | Leontowich, Adam | |
| dc.contributor.author | Thompson, Daphne | |
| dc.contributor.author | Dahn, J. R. | |
| dc.date.accessioned | 2025-07-01T23:30:34Z | |
| dc.date.available | 2025-07-01T23:30:34Z | |
| dc.date.issued | 2025-06 | |
| dc.description.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. | |
| dc.description.sponsorship | The authors thank NSERC and Tesla Canada for the funding under the auspices of the Alliance Grants program. The in-situ XRD experiments described in this paper were performed at the Canadian Light Source, a national research facility of the University of Saskatchewan, which was supported by the Canada Foundation for Innovation (CFI), the Natural Sciences and Engineering Research Council (NSERC), the Canadian Institutes of Health Research (CIHR), the Government of Saskatchewan, and the University of Saskatchewan. Svena Yu thanks the funding from Nova Scotia Graduate Scholarship Program, NSERC Postgraduate Scholarship-Doctorate Program, the President's Award and the Student Travel Support Grant from the Canadian Light Source. | |
| dc.description.version | Peer Reviewed | |
| dc.identifier.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 | |
| dc.identifier.doi | https://doi.org/10.1002/smtd.202500632 | |
| dc.identifier.uri | https://hdl.handle.net/10388/17043 | |
| dc.language.iso | en | |
| dc.publisher | Wiley | |
| dc.rights | Attribution-NonCommercial-NoDerivs 2.5 Canada | en |
| dc.rights.uri | http://creativecommons.org/licenses/by-nc-nd/2.5/ca/ | |
| dc.subject | all-dry synthesis | |
| dc.subject | LiOH NMC631 | |
| dc.subject | low temperature | |
| dc.title | In-Situ Heating X-Ray Diffraction of LiNi0.6Mn0.3Co0.1O2 and LiNi0.7Mn0.3O2 Made Using the All-Dry Synthesis Process | |
| dc.type | Article |