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Abstract All‐solid‐state sodium ion batteries (AS³iBs) are highly sought after for stationary energy storage systems due to their suitable safety and stability over a wide temperature range. Hard carbon (HC), which is low cost, exhibits a low redox potential, and a high capacity, is integral to achieve a practical large‐scale sodium‐ion battery. However, the energy density of the battery utilizing this anode material is hampered by its low initial Coulombic efficiency (ICE). Herein, two strategies, namely i) additional pyrolysis and ii) presodiation by thermal decomposition of NaBH₄, are explored to improve the ICE of pristine HC. Raman spectroscopy, X‐ray photoelectron spectroscopy, and electrochemical characterizations elucidate that the thermal treatment increases the C_sp2content in the HC structure, while the presodiation supplies the sodium to occupy the intrinsic irreversible sites. Consequently, presodiated HC exhibits an outstanding ICE (>99%) compared to the thermally treated (90%) or pristine HC (83%) in half‐cell configurations. More importantly, AS³iB using presodiated HC and NaCrO₂as the anode and cathode, respectively, exhibits a high ICE of 92% and an initial discharge energy density of . 

Abstract All‐solid‐state batteries are emerging as potential successors in energy storage technologies due to their increased safety, stemming from replacing organic liquid electrolytes in conventional Li‐ion batteries with less flammable solid‐state electrolytes. However, all‐solid‐state batteries require precise control over cycling pressure to maintain effective interfacial contacts between materials. Traditional uniaxial cell holders, often used in battery research, face challenges in accommodating electrode volume changes, providing uniform pressure distribution, and maintaining consistent pressure over time. This study introduces isostatic pouch cell holders utilizing air as pressurizing media to achieve uniform and accurately regulated cycling pressure. LiNi_0.8Co_0.1Mn_0.1O₂| Li₆PS₅Cl | Si pouch cells are fabricated and tested under 1 to 5 MPa pressures, revealing improved electrochemical performance with higher cycling pressures, with 2 MPa as the minimum for optimal operation. A bilayer pouch cell with a theoretical capacity of 100 mAh, cycled with an isostatic pouch cell holder, demonstrated a first‐cycle Coulombic efficiency of 76.9% and a discharge capacity of 173.6 mAh g⁻¹(88.1 mAh), maintaining 83.6% capacity after 100 cycles. These findings underscore the effectiveness of isostatic pouch cell holders in enhancing the performance and practical application of all‐solid‐state batteries.