Determination of Spinel Content in Cycled Li1.2Ni0.13Mn0.54Co0.13O2 Using Three-Dimensional Electron Diffraction and Precession Electron Diffraction Article Swipe
Matthias Quintelier
,
Tyché Perkisas
,
Romy Poppe
,
Maria Batuk
,
Mylène Hendrickx
,
Joke Hadermann
·
YOU?
·
· 2021
· Open Access
·
· DOI: https://doi.org/10.3390/sym13111989
YOU?
·
· 2021
· Open Access
·
· DOI: https://doi.org/10.3390/sym13111989
Among lithium battery cathode materials, Li1.2Ni0.13Mn0.54Co0.13O2 (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.
Related Topics
Concepts
Electron diffraction
Spinel
Materials science
Diffraction
Crystal twinning
Reflection high-energy electron diffraction
Selected area diffraction
Phase (matter)
Transmission electron microscopy
Stacking
Crystallography
Optics
Chemistry
Nuclear magnetic resonance
Nanotechnology
Physics
Microstructure
Composite material
Metallurgy
Organic chemistry
Metadata
- Type
- article
- Language
- en
- Landing Page
- https://doi.org/10.3390/sym13111989
- https://www.mdpi.com/2073-8994/13/11/1989/pdf?version=1635905891
- OA Status
- gold
- Cited By
- 6
- References
- 46
- Related Works
- 10
- OpenAlex ID
- https://openalex.org/W3206177569
All OpenAlex metadata
Raw OpenAlex JSON
- OpenAlex ID
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https://openalex.org/W3206177569Canonical identifier for this work in OpenAlex
- DOI
-
https://doi.org/10.3390/sym13111989Digital Object Identifier
- Title
-
Determination of Spinel Content in Cycled Li1.2Ni0.13Mn0.54Co0.13O2 Using Three-Dimensional Electron Diffraction and Precession Electron DiffractionWork title
- Type
-
articleOpenAlex work type
- Language
-
enPrimary language
- Publication year
-
2021Year of publication
- Publication date
-
2021-10-20Full publication date if available
- Authors
-
Matthias Quintelier, Tyché Perkisas, Romy Poppe, Maria Batuk, Mylène Hendrickx, Joke HadermannList of authors in order
- Landing page
-
https://doi.org/10.3390/sym13111989Publisher landing page
- PDF URL
-
https://www.mdpi.com/2073-8994/13/11/1989/pdf?version=1635905891Direct link to full text PDF
- Open access
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YesWhether a free full text is available
- OA status
-
goldOpen access status per OpenAlex
- OA URL
-
https://www.mdpi.com/2073-8994/13/11/1989/pdf?version=1635905891Direct OA link when available
- Concepts
-
Electron diffraction, Spinel, Materials science, Diffraction, Crystal twinning, Reflection high-energy electron diffraction, Selected area diffraction, Phase (matter), Transmission electron microscopy, Stacking, Crystallography, Optics, Chemistry, Nuclear magnetic resonance, Nanotechnology, Physics, Microstructure, Composite material, Metallurgy, Organic chemistryTop concepts (fields/topics) attached by OpenAlex
- Cited by
-
6Total citation count in OpenAlex
- Citations by year (recent)
-
2025: 3, 2024: 2, 2022: 1Per-year citation counts (last 5 years)
- References (count)
-
46Number of works referenced by this work
- Related works (count)
-
10Other works algorithmically related by OpenAlex
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