This study investigates lyocell-based activated carbon fibers (ACFs) for their suitability in adsorbing and electrochemically detecting toxic HCl gas. ACFs were prepared via steam activation, varying temperature (800–900 °C) and time (40–240 min) to assess their adsorption and sensing capabilities. The adjustment of activation temperature and reaction time aimed to regulate the uniformity of the pore structure and pore size of the active reaction area, as well as the number of reaction sites in the ACFs. Optimal ACFs were achieved at 900 °C for 50 min, exhibiting the highest specific surface area (1403 m2/g) and total pore volume (0.66 cm3/g). Longer reaction times resulted in pore formation and disorder, reducing mechanical strength. The ACFs prepared under optimal conditions demonstrated a rapid increase in resistance during sensor measurement, indicating a significant sensitivity to HCl gas. These findings suggest the potential of ACFs for efficient HCl gas adsorption (1626.20 mg/g) and highlight the importance of activation parameters in tailoring their properties for practical applications.