Publication date: 15th December 2025
Emerging and safer rechargeable battery technologies such as sodium-ion batteries have attracted much attention in recent years due to the low cost and large natural abundance of sodium sources. Non-graphitic hard carbons (HC), formed by randomly orientated and curved graphene sheets with expanded interlayer distance (3.6–4 Å) and with the possibility of being derived from biosources, are promising anode candidates for Na-ion batteries, showing typical reversible capacities of ca. 300 mAh g−1. The reaction mechanisms that drive the sodiation/desodiation properties in hard carbons are complex and relate to (1) Na+ ion adsorption at edge sites and defects, (2) Na+ intercalation into graphene–graphene interlayer spacing, and (3) Na+ ion insertion into nanopores. These storage mechanisms and their subsequent electrochemical response are strictly linked to the characteristic slope and plateau regions observed in the voltage profile of these materials.
In this work we show that electron paramagnetic resonance (EPR) spectroscopy is a powerful and fast diagnostic tool to predict the extent of the charge stored in the slope and plateau regions during galvanostatic tests in pristine hard carbon materials. EPR lineshape simulation and temperature-dependent measurements help to separate the nature of the spins in mechanochemically modified hard carbon materials synthesised at different temperatures. This proves relationships between structure modification and electrochemical signatures in the galvanostatic curves to obtain information on their sodium storage mechanism. Furthermore, we show through the use of ex-situ EPR the evolution of these EPR signals at different states of charge to further elucidate the storage mechanisms in these hard carbons, to answer questions related to the nature of the Na clusters.
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