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The research proposed a novel method of obtaining sorption material from readily available Acorus calamus biomass through a combination of physical and chemical activation processes. The material with the highest specific surface area (1652 m2 g−1) was obtained by physical activation with CO 2 , followed by chemical activation with KOH. Reversing the order of activation methods resulted in a lower specific surface area (1014 m2 g−1) of the carbon sample. Chemical activation produced activated carbon with a surface area of 1066 m2 g−1-, while physical activation produced 390 m2 g−1. This confirms the synergistic effect of combining the two activation methods for biocarbon. It was observed that physical activation with CO 2 generates a diverse range of pores, including meso- and macropores, while chemical activation induces the formation of micropores. In contrast, reversing the order of these processes leads to the degradation of the porous structure. The application of physical-chemical activation with synergistic effects represents a significant advancement in producing high-quality activated biocarbon for various applications, such as wastewater treatment and energy storage. The combination of the two activation methods resulted in a synergistic effect, leading to the production of carbon material of higher quality. Additionally, the diversified pore sizes will enable the sorption of various pollutants in the aquatic environment and air pollutants, where gas particles are much smaller. [Display omitted] • New highly porous sorption materials from Acorus calamus biomass. • The novel method of preparation sorption carbon material. • A new synergistic effect of two activation method was described. • Preparation of material with various pore sizes in a new way. • A mechanism for porous structure development during activation was proposed. [ABSTRACT FROM AUTHOR]