Box-Behnken design for the synthesis optimization of mesoporous sulfur-doped carbon-based materials from birch waste: Promising candidates for environmental and energy storage application

The development of biomass-based carbon materials has accelerated the research interest in environmental (e.g., adsorbents for wastewater decontamination) and energy applications (e.g., batteries). In this paper, we developed a series of carbon materials (CMs) using a sulfur doping strategy to improve the physicochemical, adsorptive and energy storage properties of the aforementioned CMs. CMs were prepared and optimized using an experimental design denoted as the Box-Behnken design approach with three independent factors (i.e., the temperature of pyrolysis, zinc chloride: biomass ratio and sulfur: biomass ratio), and the responses were evaluated, namely the Specific Surface Area (S _BET), mesopore area (A _Meso) and micropore area (A _Micro) with the help of Nitrogen Physisorption. According to the statistical analysis, under the studied conditions, the responses were mainly influenced by the pyrolysis temperature and ZnCl ₂ ratio, while the sulfur content did not give rise to any remarkable differences in the selected responses. The physicochemical characterization of the CMs suggested that very high Specific Surface Areas ranging from 1069 to 1925 m ² g ⁻¹ were obtained. The sulfur doping resulted in up to 7.33 wt% of sulfur in the CM structure, which yielded CMs with more defects and hydrophilic surfaces. When tested as adsorbents, CMs exhibited a very high adsorption capacity (190 – 356 mg g ⁻¹), and as anodes, they demonstrated a competitive Lithium Ion Battery (LIB) storage capacity, at least during the first five cycles (306 mAhg ⁻¹ at 1 C for CM9). However, further studies on long-term cyclability are required to prove the CM materials suitability in LIBs. This work extends our understanding of how pyrolysis and sulfur doping of biomass feedstock affects carbon materials' usability, final characteristics and potential to use in wastewater decontamination by adsorption and as anodes in LIBs.