Solution treatment effect on precipitates, microstructure, and properties of S32707 hyper-duplex stainless steel
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摘要: 通過Thermo-Calc熱力學計算、OM和FE-SEM觀察、力學性能和腐蝕性能試驗對不同固溶溫度下的特超級雙相不銹鋼進行分析和研究。結果表明：σ相和非平衡氮化物是固溶水冷組織中的主要析出相，當固溶溫度低于1050 ℃時，σ相優先沿雙相界面析出，顯著降低雙相不銹鋼的沖擊韌性；當固溶溫度高于1100 ℃，非平衡氮化物開始在鐵素體晶粒內部析出，且隨著固溶溫度的升高，非平衡氮化物析出數量增加。這是由于固溶水冷過程中氮在鐵素體中的溶解度快速降低，過飽和的氮來不及擴散到相鄰奧氏體中，只能以氮化物的形式析出。隨固溶溫度升高，鐵素體含量增加，奧氏體含量降低，實驗鋼的強度增加，沖擊韌性降低。在1080～1120 ℃之間固溶時，雙相比例接近1∶1，S32707特超級雙相不銹鋼具有優良的綜合力學性能和耐晶間腐蝕性能。Abstract: Duplex stainless steel (DSS) has been widely used in some harsh environments, such as flue gas shedding and seawater desalination, because of its high strength and corrosion resistance. These excellent properties rely on a high alloy content (Cr, Mo, N, etc.) and perfect dual-phase equilibrium. The dual-phase equilibrium mainly includes dual-phase proportion balance, properties balance, and absence of clear secondary phase in the solid solution structure. As one of the main developmental directions of DSS, hyper-duplex stainless steel (HDSS) has attracted much attention in recent years. In this paper, the effects of solution treatment on precipitates, microstructure, and properties of S32707 HDSS were studied by Thermo-Calc thermodynamic calculation, OM and FE-SEM observation, mechanical properties, and corrosion property tests. The results showed that σ phase and non-equilibrium nitrides were the main precipitates of solution-treated HDSS. When the solution temperature was lower than 1050 ℃, the σ phase precipitated preferentially along the dual-phase boundaries, which significantly reduced the impact toughness of HDSS. When the solution temperature was higher than 1100 ℃, non-equilibrium nitrides precipitated in ferrite grains, and the number of non-equilibrium nitrides increased with an increase in solution temperature. The reason for the non-equilibrium nitride precipitation was that the nitrogen content in the ferrite increased with an increase in temperature. This led to the supersaturation of nitrogen in the ferrite grains during the rapid cooling process. Under such conditions, the finely dispersed non-equilibrium nitrides precipitated in the ferrite grains. With increasing solution temperature, the content of the ferrite increased, the content of austenite decreased, the strength increased, and the impact toughness decreased. The optimal solution temperature of HDSS was 1080?1120 ℃. Under this condition, the ratio of duplex was close to 1∶1, and the S32707 hyper duplex stainless steel presented excellent comprehensive mechanical properties and intergranular corrosion resistance.
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圖 1 實驗鋼鍛后組織。（a）縱向；（b）橫向
Figure 1. Structure of the tested steel being forged: (a) longitudinal; (b) transverse
圖 2 實驗鋼Thermo-Calc熱力學計算結果
Figure 2. Thermo-Calc thermodynamic calculation of tested steel
圖 3 不同固溶溫度下析出相、組織光鏡形貌及雙相統計結果。（a）1000 ℃；（b）1050 ℃；（c）1100 ℃；（d）1150 ℃；（e）1200 ℃；（f）1250 ℃；（g）1300 ℃；（h）雙相統計結果
Figure 3. OM images of precipitates and microstructure at different annealing temperatures and results of dual-phase volume fractions: (a) 1000 ℃; (b) 1050 ℃; (c) 1100 ℃; (d) 1150 ℃; (e) 1200 ℃; (f) 1250 ℃; (g) 1300 ℃; (h) results of dual-phase volume fractions at different annealing temperatures
圖 4 不同固溶溫度下析出相和組織的背散射電子形貌。（a）1000 ℃；（b）1050 ℃；（c）1080 ℃
Figure 4. Backscattered electron observation of precipitates and microstructure at different annealing temperatures: (a) 1000 ℃; (b) 1050 ℃; (c) 1080 ℃
圖 5 不同固溶溫度下非平衡氮化物OM形貌。（a）1080 ℃；（b）1100 ℃；（c）1150 ℃；（d）1200 ℃；（e）1250 ℃；（f）1300 ℃
Figure 5. OM observation of non-equilibrium nitrides at different annealing temperatures: (a) 1080 ℃; (b) 1100 ℃; (c) 1150 ℃; (d) 1200 ℃; (e) 1250 ℃; (f) 1300 ℃
圖 6 非平衡氮化物TEM形貌（a）和選區電子衍射（b），不同溫度下氮在鐵素體和奧氏體中含量的熱力學計算結果（c）
Figure 6. TEM morphology (a) and electron selected area diffraction (b) of nonequilibrium nitride, thermodynamic calculation results (c) of N content in ferrite and austenite at different temperatures
圖 7 不同固溶溫度下實驗鋼拉伸斷口FE-SEM形貌。（a）1050 ℃；（b）1080 ℃；（c）1100 ℃；（d）1120 ℃；（e）1150 ℃；（f）1200 ℃
Figure 7. FE-SEM observation of tensile fracture of tested steel at different annealing temperatures: (a) 1050 ℃; (b) 1080 ℃; (c) 1100 ℃; (d) 1120 ℃; (e) 1150 ℃; (f) 1200 ℃
圖 8 不同固溶溫度下實驗鋼晶間腐蝕宏觀與OM形貌
Figure 8. Macro and OM morphology of experimental steel after an intergranular corrosion test at different annealing temperatures
表 1 實驗鋼化學成分（質量分數）
Table 1. Chemical composition of the tested steel
% C Si Mn Cr Mo Ni N Cu Co Fe 0.01 0.37 1.18 27.42 4.64 6.50 0.34 0.54 0.77 Bal. 
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表 2 不同固溶溫度下實驗鋼力學性能
Table 2. Mechanical properties of experimental steel at different annealing temperatures
Annealing temperature /
℃Tensile
strength /
MPaYield
strength /
MPaElongation/
%Impact
energy /
J1050 944 701 31 153 1080 938 719 39 232 1100 941 724 38 223 1120 936 729 35 219 1150 940 736 35 195 1200 953 757 30 163 ASTM A790/A790M ≥920 ≥700 ≥25
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