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The mechanism of brittleness of Ml52 martensitic heat resistant steel due to slow cooling during quenching was experimentally investigated. The mechanical property tests and microstructure observation were conducted by TEM and XRD. The results showed that the presence of irreversible brittleness during slow cooling of quenching for Ml 52 steel is attributed to the continuous M23C6 precipitation along prior austenite grain boundaries and M2C along prior residual austenite film. The residual austenite in the steel was unstable and decomposed after the precipitation of second phase during the process of slow cooling of quenching. The low cooling rate within the temperature range from 820 ℃ to 660 ℃ plays a key role in impact toughness, and the precipitation of second phase in the same temperature range results in irreversible brittleness.

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