Bastos, Tarso Leandroda Silva, Camila CristinaNunes, DanielaFortunato, ElviraMartins, RodrigoKathan, DevadharshiniMustain, William EarlGelamo, Rogério ValentimColmati, Flavio2026-02-032026-02-032025-11-182574-0970PURE: 151944160PURE UUID: 8a20b935-bad8-49e0-b4d1-872628498cb1Scopus: 105023374490WOS: 001618347800001ORCID: /0000-0002-4202-7047/work/204628453ORCID: /0000-0003-3115-6588/work/204630170http://hdl.handle.net/10362/199982Publisher Copyright: © 2025 The Authors. Published by American Chemical SocietyMultilayer graphene (MLG) was obtained by 3 h ultrasonication of thermally expanded graphite in n-propanol, producing 5–13-nm-thick flakes with 1–50 μm lateral size. The powder was dry-pressed into self-supported disk electrodes (MLGD) and surface-activated by brief MW-PECVD and RF-PECVD in Ar/CO2 and Ar/O2. PECVD raised Raman ID /IG from 0.07 to 0.26–0.28 (La ≈ 275 → 69–92 nm) and gave higher localized O for CO2 MW-PECVD (≈1.05 wt % vs ≈0.13 wt % for O2). Electrochemically, areal capacitance increased ≈11.9 → ≈16.5 mF·cm–2 (∼39%), and ethanol oxidation peak currents improved up to ≈ 40% (peak up to 2.94 mA·cm–2 for O2 RF-PECVD in 1.0 M NaOH + 2.0 M EtOH), with >95% capacitance retention after 15 CV cycles. These results highlight that PECVD post-treatment provides a rapid, reagent-free, and tunable surface functionalization of compacted MLG electrodes, enabling increased capacitance and enhanced ethanol oxidation with minimal bulk structural degradation.195641864engAr/CO and Ar/O glow dischargesEthanol oxidationPECVDPlasma processSurface functionalizationGeneral Materials ScienceMetal-Free Multilayer Graphene Electrodes Activated by PECVD for Electrochemical Oxidation Enhancementjournal article10.1021/acsanm.5c03602https://www.scopus.com/pages/publications/105023374490https://www.webofscience.com/wos/woscc/full-record/WOS:001618347800001