Morphological and Structural Analysis of Pyrolytic Carbon from Simple Thermal Methane Pyrolysis

This study presents a comprehensive morphological and structural analysis of carbon materials produced via simple thermal methane pyrolysis conducted under laboratory conditions in a quartz reactor without the use of catalysts. The process, carried out at 1000 °C, achieved moderate methane conversion (36.5%), process efficiency (36.1%), and very high selectivity (98.9%) towards hydrogen production, highlighting its potential as a CO2-free hydrogen generation method. Distinct carbon morphologies were observed depending on the formation areas within the reactor: a predominant flake-like silver carbon formed on reactor walls at temperatures between 600 and 980 °C (accounting for 91% of the solid product) and a minor powdery carbon formed near 980–1000 °C (9% of the solids). The powdery carbon exhibited a high specific surface area (125.3 m2/g), substantial mesoporosity (60%), and porous spherical aggregates, indicating an amorphous structure. In contrast, flake-like carbon demonstrated a low surface area (1.99 m2/g), high structural order confirmed by Raman spectroscopy, and superior thermal stability, making it suitable for advanced applications requiring mechanical robustness. Additionally, polycyclic aromatic hydrocarbons were detected in cooler zones of the reactor, suggesting side reactions in low-temperature areas. The study underscores the impact of temperature zones on carbon structure and properties, emphasizing the importance of precise thermal control to tailor carbon materials for diverse industrial applications while producing clean hydrogen.