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The key technological implementation of sodium-ion batteries is converting biomass-derived hard carbons into effective anode materials. This becomes feasible if appropriate knowledge of the relations between the structure of carbonized biomass products, the mineral ash content in them, and Na storage properties is gained. In this study, we examine the simultaneous impact of the ash phase composition and carbon structure on the Na storage properties of hard carbons derived from spent coffee grounds (SCGs). The carbon structure is modified using the pre-carbonization of SCGs at 750 °C, followed by annealing at 1100 °C in an Ar atmosphere. Two variants of the pre-carbonization procedure are adopted: the pre-carbonization of SCGs in a fixed bed and CO2 flow. For the sake of comparison, the pre-carbonized products are chemically treated to remove the ash content. The Na storage performance of SCG-derived carbons is examined in model two and three Na-ion cells. It was found that ash-containing carbons outperformed the ash-free analogs with respect to cycling stability, Coulombic efficiency, and rate capability. The enhanced performance is explained in terms of the modification of the carbon surface by ash phases (mainly albite) and its interaction with the electrolyte, which is monitored by ex situ XPS. [ABSTRACT FROM AUTHOR]