Waste Tire Heat Treatment to Prepare Sulfur Self-Doped Char: Operando Insight into Activation Mechanisms Based on the Char Structures Evolution

Waste tire (WT) can be heat-treated to be high-quality sulfur self-doped char via pyrolysis and K2FeO4-assisted activation processes. This work aimed at further studying the activation mechanisms based on the char structures evolution by operando experimental method. Activation treatment process (from 50 °C to 800 °C and then held for 3 h) was divided into six typical stages (S1–S6) and consisted of carbonization process (S1–S4) and effective activation process (S4–S6). During the carbonization process, the specific capacitance only increased from 0.2 F/g to 12.4 F/g, aromatic ring systems and alkyl-aryl C-C bonds generated, S 2p3/2 (sulphide bridge) was mainly gradually consumed. During the effective activation process, the specific capacitance hugely increased from 12.4 F/g to 112.5 F/g, aromatic ring systems and alkyl-aryl C-C bonds turned to ordered graphitic char. The pores massively generated from S4 to S5, while micropores partly formed to larger and mesopores+macropores fractionally converting to smaller from S5 to S6. Besides, both S 2p3/2 and S 2p5/2 (sulphone bridge) were enriched after S5. Furthermore, the key structural parameters for huge improvement of specific capacitance were found and it further revealed that mesopores+macropores possessed stronger promotion effect than micropores and S 2p3/2 was more beneficial than S 2p5/2.