Sustainable Carbon Source from Almond Shell Waste: Synthesis, Characterization, and Electrochemical Properties

This study demonstrates the complete transformation of almond shell waste into a high-performance carbon material for carbon paste electrode (CPE) fabrication. The biocarbon was synthesized via carbonization at 800 °C and subsequently activated with CO₂, resulting in a semicrystalline structure rich in carbonyl groups-consistent with its lignocellulosic origin (34.25% cellulose, 13.48% hemicellulose, 48.03% lignin). Carbonization increased the total pore volume of carbonized almond (CAR_ALD) by nearly 13-fold and the specific surface area by over two orders of magnitude compared to raw almond (RAW_ALD), while CO₂ activation further enhanced activated almond's (ACT_ALD) surface area (~19%) and pore volume (~35%). To improve electrochemical performance, Bi₂O₃ doped with Sm was applied as a surface modifier. Comprehensive characterization (N₂ physisorption X-Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopic Analysis (FTIR), X-Ray Photoelectron Spectroscopic Analysis (XPS), Thermogravimetric and Differential Thermal Analysis (TG-DTA), Cyclic voltammetry (CV), Electrochemical impedance spectroscopy (EIS)) confirmed the material's structural integrity, graphitic features, and successful modifier incorporation. Electrochemical testing revealed the highest current response (48 µA) for the CPE fabricated from CAR_ALD/Bi₂O₃-Sm, indicating superior electrocatalytic activity and reduced charge transfer resistance. Notably, this is the first report of a fully functional CPE working electrode fabricated entirely from waste material.