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EELS Probing of lithium based 2-D battery compounds processed by liquid phase exfoliation

Abstract number: 5853

Session Code: IM08-412

DOI: 10.1002/9783527808465.EMC2016.5853

Meeting: The 16th European Microscopy Congress 2016

Session: Instrumentation and Methods

Topic: Spectromicroscopies and analytical microscopy (electrons and photons, experiment and theory)

Presentation Form: Poster

Corresponding Email: poklea@tcd.ie

Anuj Pokle (1), João Coelho (2), Eva Macguire (3), Clive Downing (4), Patrick Casey (5), Cormac McGuinness (3), Valeria Nicolosi (5)

1. Advance Microscopy Lab, Trinity College Dublin, Dublin, Irlande 2. Chemistry, Trinity College Dublin, Dublin, Irlande 3. Physics, Trinity College Dublin, Dublin, Irlande 4. AML, Trinity College Dublin, Dublin, Irlande 5. CRANN, Trinity College Dublin, Dublin, Irlande

Keywords: 2D materials, battery, EELS, ELNES, liquid phase exfoliation, lithium

Two-dimensional lithiated nanosheets usually show excellent electrochemical performance due to an increase in surface area and shorter diffusion paths. However, processing techniques, such as shear mixing or liquid phase exfoliation could induce phase changes or knock out some of the structural lithium (Li) ions, what in turn might result in poor electrochemical performance. Here different lithiated layered compounds mainly LiCoO2, LiMn2O4, and Li5Ti4O12 were chemically exfoliated and investigated using electron energy loss spectroscopy (EELS) for their Li-K edge. Further analyses were carried out, looking at the oxygen (O) K edge with their respective transition metal core loss peak (Mn, Co and Ti) which revealed changes in the Energy loss near edge structures (ELNES) when compared to the unlithiated compounds. STEM-EELS analyses confirmed uneven distribution of lithium within the lithiated layered materials. In this work, EELS was used for the first time to detect and to probe the chemical environment of the lithium in liquid phase exfoliated material. 

Figures:

(a, b) shows O K-edge and Co L-edge of LiCoO2 respectively. (c,d) Li-K edge and Ti-L/O-K edge respectively for Li4Ti5O12, (e and f) O-K edge and Mn-L edge respectively of LiMn2O4.

(a) Bright field TEM image of a flake of LiCoO2. The TEM beam was condensed to a diameter of approximately 10nm and EELS spectra were collected from regions marked A and B. (b) EELS spectra collected from the regions marked A and B in (a). The lithium signal is clearly present in the spectrum collected from the centre of the flake, while it is absent from the spectrum collected from the edge. (c) The percentage of flakes in which a lithium signal was detected for each centrifugation speed. (e) The EELS spectrum collected from a LiCoO2 flake (d) as the flake remains illuminated by the beam over a period of four minutes. The lithium signal is clearly visible in the first spectrum and decreases over time until it is completely absent.

The EELS signals of all the materials examined showing the presence lithium (red arrows). Other reference spectra of MnO2, cobalt oxide and titanium oxide

To cite this abstract:

Anuj Pokle, João Coelho, Eva Macguire, Clive Downing, Patrick Casey, Cormac McGuinness, Valeria Nicolosi; EELS Probing of lithium based 2-D battery compounds processed by liquid phase exfoliation. The 16th European Microscopy Congress, Lyon, France. https://emc-proceedings.com/abstract/eels-probing-of-lithium-based-2-d-battery-compounds-processed-by-liquid-phase-exfoliation/. Accessed: February 23, 2019
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