Multicycle operando Raman spectroscopy reveals reversible and irreversible transitions in LiNiO2electrodes

del Campo Ortiz, E ORCID: 0000-0001-7508-8471, Neale, AR ORCID: 0000-0001-7675-5432, Sonni, M ORCID: 0000-0001-6872-445X, Daniels, LM ORCID: 0000-0002-7077-6125, Zukowska, GZ, Rosseinsky, MJ ORCID: 0000-0002-1910-2483, Marcinek, M and Hardwick, LJ ORCID: 0000-0001-8796-685X (2026) Multicycle operando Raman spectroscopy reveals reversible and irreversible transitions in LiNiO2electrodes Physical Chemistry Chemical Physics, 28 (1). pp. 112-119. ISSN 1463-9076, 1463-9084

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Abstract

Operando Raman spectroscopy of the delithiation and lithiation of LiNiO<inf>2</inf> positive electrodes is reported over the first three cycles. Optimisation of the operando electrochemical Raman cell configuration facilitated the characterisation of composite electrodes across multiple cycles with high relevance for practical Li-ion cell chemistry. Tracking the E<inf>g</inf> and A<inf>1g</inf> Raman modes highlighted localised irreversible changes, particularly correlated to first-cycle inefficiencies in LiNiO<inf>2</inf>, followed by reversible band shifts and intensity changes upon subsequent cycles. Furthermore, trends in both the band position and intensities were related to the state of lithiation (x(Li) in Li<inf>x</inf>NiO<inf>2</inf>) and the phase transitions through hexagonal and monoclinic phases (H1, M, H2 and H3).

Item Type:	Article
Uncontrolled Keywords:	34 Chemical Sciences, 3406 Physical Chemistry, 40 Engineering, 51 Physical Sciences, 4016 Materials Engineering
Divisions:	Faculty of Science & Engineering Faculty of Science & Engineering > School of Physical Sciences Faculty of Science & Engineering > School of Physical Sciences > Chemistry
Depositing User:	Symplectic Admin
Date Deposited:	18 Nov 2025 10:50
Last Modified:	28 Feb 2026 13:39
DOI:	10.1039/d5cp03622d
Open Access URL:	https://pubs.rsc.org/en/content/articlehtml/2025/c...
Related Websites:	Author Publisher
URI:	https://livrepository.liverpool.ac.uk/id/eprint/3195485
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