The evolution of microstructure and mechanical properties of 310S austenitic stainless steel and GH3536 nickel-based alloy in hydrogen metallurgy service condition is investigated by conducting heat treatment under high temperature and hydrogen atmosphere. As the annealing time increases at 750 °C, carbide precipitate phases of the σ and μ brittle phases appear in the materials. At 900 °C, the dissolution of carbides induces the dispersion of brittle phases, while the hydrogen content reaching its peak. These brittle phases are still present at defects like grain boundaries at 1050 °C, with the surface of precipitates showing corrosion pits. Materials exhibit increasing strength and hardness initially with temperature and annealing time, followed by a decrease. Meanwhile, fracture elongation shows a positive correlation with temperature but a negative correlation with time. After annealing at 1050 °C for 500 h, GH3536 retains its high-temperature softening behavior and elongation at fracture, demonstrating excellent plastic stability. Furthermore, the mechanism of high temperature and hydrogen affecting metals is expounded, providing reference for the selection and optimization of materials which service in high temperature and hydrogen.
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