Determination of Spinel Content in Cycled Li<sub>1.2</sub>Ni<sub>0.13</sub>Mn<sub>0.54</sub>Co<sub>0.13</sub>O<sub>2</sub> Using Three-Dimensional Electron Diffraction and Precession Electron Diffraction
Among lithium battery cathode materials, Li<sub>1.2</sub>Ni<sub>0.13</sub>Mn<sub>0.54</sub>Co<sub>0.13</sub>O<sub>2</sub> (LR-NMC) has a high theoretical capacity, but suffers from voltage and capacity fade during cycling. This is partially...
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oai:doaj.org-article:d6053cd5d0134d67a13578782a0722752021-11-25T19:05:49ZDetermination of Spinel Content in Cycled Li<sub>1.2</sub>Ni<sub>0.13</sub>Mn<sub>0.54</sub>Co<sub>0.13</sub>O<sub>2</sub> Using Three-Dimensional Electron Diffraction and Precession Electron Diffraction10.3390/sym131119892073-8994https://doaj.org/article/d6053cd5d0134d67a13578782a0722752021-10-01T00:00:00Zhttps://www.mdpi.com/2073-8994/13/11/1989https://doaj.org/toc/2073-8994Among lithium battery cathode materials, Li<sub>1.2</sub>Ni<sub>0.13</sub>Mn<sub>0.54</sub>Co<sub>0.13</sub>O<sub>2</sub> (LR-NMC) has a high theoretical capacity, but suffers from voltage and capacity fade during cycling. This is partially ascribed to transition metal cation migration, which involves the local transformation of the honeycomb layered structure to spinel-like nano-domains. Determination of the honeycomb layered/spinel phase ratio from powder X-ray diffraction data is hindered by the nanoscale of the functional material and the domains, diverse types of twinning, stacking faults, and the possible presence of the rock salt phase. Determining the phase ratio from transmission electron microscopy imaging can only be done for thin regions near the surfaces of the crystals, and the intense beam that is needed for imaging induces the same transformation to spinel as cycling does. In this article, it is demonstrated that the low electron dose sufficient for electron diffraction allows the collection of data without inducing a phase transformation. Using calculated electron diffraction patterns, we demonstrate that it is possible to determine the volume ratio of the different phases in the particles using a pair-wise comparison of the intensities of the reflections. Using this method, the volume ratio of spinel structure to honeycomb layered structure is determined for a submicron sized crystal from experimental three-dimensional electron diffraction (3D ED) and precession electron diffraction (PED) data. Both twinning and the possible presence of the rock salt phase are taken into account. After 150 charge–discharge cycles, 4% of the volume in LR-NMC particles was transformed irreversibly from the honeycomb layered structure to the spinel structure. The proposed method would be applicable to other multi-phase materials as well.Matthias QuintelierTyché PerkisasRomy PoppeMaria BatukMylene HendrickxJoke HadermannMDPI AGarticle3D EDPEDNMCphase ratiobatteryMathematicsQA1-939ENSymmetry, Vol 13, Iss 1989, p 1989 (2021) |
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3D ED PED NMC phase ratio battery Mathematics QA1-939 |
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3D ED PED NMC phase ratio battery Mathematics QA1-939 Matthias Quintelier Tyché Perkisas Romy Poppe Maria Batuk Mylene Hendrickx Joke Hadermann Determination of Spinel Content in Cycled Li<sub>1.2</sub>Ni<sub>0.13</sub>Mn<sub>0.54</sub>Co<sub>0.13</sub>O<sub>2</sub> Using Three-Dimensional Electron Diffraction and Precession Electron Diffraction |
| description |
Among lithium battery cathode materials, Li<sub>1.2</sub>Ni<sub>0.13</sub>Mn<sub>0.54</sub>Co<sub>0.13</sub>O<sub>2</sub> (LR-NMC) has a high theoretical capacity, but suffers from voltage and capacity fade during cycling. This is partially ascribed to transition metal cation migration, which involves the local transformation of the honeycomb layered structure to spinel-like nano-domains. Determination of the honeycomb layered/spinel phase ratio from powder X-ray diffraction data is hindered by the nanoscale of the functional material and the domains, diverse types of twinning, stacking faults, and the possible presence of the rock salt phase. Determining the phase ratio from transmission electron microscopy imaging can only be done for thin regions near the surfaces of the crystals, and the intense beam that is needed for imaging induces the same transformation to spinel as cycling does. In this article, it is demonstrated that the low electron dose sufficient for electron diffraction allows the collection of data without inducing a phase transformation. Using calculated electron diffraction patterns, we demonstrate that it is possible to determine the volume ratio of the different phases in the particles using a pair-wise comparison of the intensities of the reflections. Using this method, the volume ratio of spinel structure to honeycomb layered structure is determined for a submicron sized crystal from experimental three-dimensional electron diffraction (3D ED) and precession electron diffraction (PED) data. Both twinning and the possible presence of the rock salt phase are taken into account. After 150 charge–discharge cycles, 4% of the volume in LR-NMC particles was transformed irreversibly from the honeycomb layered structure to the spinel structure. The proposed method would be applicable to other multi-phase materials as well. |
| format |
article |
| author |
Matthias Quintelier Tyché Perkisas Romy Poppe Maria Batuk Mylene Hendrickx Joke Hadermann |
| author_facet |
Matthias Quintelier Tyché Perkisas Romy Poppe Maria Batuk Mylene Hendrickx Joke Hadermann |
| author_sort |
Matthias Quintelier |
| title |
Determination of Spinel Content in Cycled Li<sub>1.2</sub>Ni<sub>0.13</sub>Mn<sub>0.54</sub>Co<sub>0.13</sub>O<sub>2</sub> Using Three-Dimensional Electron Diffraction and Precession Electron Diffraction |
| title_short |
Determination of Spinel Content in Cycled Li<sub>1.2</sub>Ni<sub>0.13</sub>Mn<sub>0.54</sub>Co<sub>0.13</sub>O<sub>2</sub> Using Three-Dimensional Electron Diffraction and Precession Electron Diffraction |
| title_full |
Determination of Spinel Content in Cycled Li<sub>1.2</sub>Ni<sub>0.13</sub>Mn<sub>0.54</sub>Co<sub>0.13</sub>O<sub>2</sub> Using Three-Dimensional Electron Diffraction and Precession Electron Diffraction |
| title_fullStr |
Determination of Spinel Content in Cycled Li<sub>1.2</sub>Ni<sub>0.13</sub>Mn<sub>0.54</sub>Co<sub>0.13</sub>O<sub>2</sub> Using Three-Dimensional Electron Diffraction and Precession Electron Diffraction |
| title_full_unstemmed |
Determination of Spinel Content in Cycled Li<sub>1.2</sub>Ni<sub>0.13</sub>Mn<sub>0.54</sub>Co<sub>0.13</sub>O<sub>2</sub> Using Three-Dimensional Electron Diffraction and Precession Electron Diffraction |
| title_sort |
determination of spinel content in cycled li<sub>1.2</sub>ni<sub>0.13</sub>mn<sub>0.54</sub>co<sub>0.13</sub>o<sub>2</sub> using three-dimensional electron diffraction and precession electron diffraction |
| publisher |
MDPI AG |
| publishDate |
2021 |
| url |
https://doaj.org/article/d6053cd5d0134d67a13578782a072275 |
| work_keys_str_mv |
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