Stress Corrosion Cracking Behavior of Nuclear Grade 316LN Stainless Steel Bend in High Temperature and Pressure Water

ZHU Ruolin1,2, ZHANG Litao1, WANG Jianqiu1,ZHANG Zhiming1, HAN En-Hou1
1 Key Laboratory of Nuclear Materials and Safety Assessment, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China
2 China Nuclear Power Operation Technology Corporation, LTD, Wuhan 430223, China
 Cite this article:
ZHU Ruolin, ZHANG Litao, WANG Jianqiu, ZHANG Zhiming, HAN En-Hou. Stress Corrosion Cracking Behavior of Nuclear Grade 316LN Stainless Steel Bend in High Temperature and Pressure Water. Journal of Chinese Society for Corrosion and Protection[J], 2018, 38(1): 54-61 doi:10.11902/1005.4537.2017.006

Abstract:
The stress corrosion crack propagation behavior of the pipe bend of nuclear grade 316LN stainless steel (SS) in high temperature high pressure water was studied by means of direct current potential drop (DCPD) method coupled with in-situ measuring the crack length of the compact tension (CT) specimen, as well as scanning electron microscope (SEM) and electron back scattering diffraction (EBSD) technique. Results indicated that the crack growth rate monotonically increased with the increase of temperature ranging from 270 ℃ to 330 ℃, and the crack growth rate at 330 ℃ was 1.7 fold of that at 270 ℃. The apparent activation energy (Eaae) for stress corrosion crack propagation of 316LN SS was 52 kJ/mol. The crack growth rate of 316LN SS was affected by the solution with dissolved 1500 mg/L B+2.3 mg/L Li in high temperature high pressure water and the influence extent depended on the pH of the solution. The results of the crack growth rates could provide data support for the plant safety evaluation and remnant life prediction. Intergranular stress corrosion cracking was observed for the fractured surface of 316LN stainless steel tested in pressurized high temperature water. The crack propagated along with the large angle grain boundaries instead of the coincidence site lattice (CSL) boundaries and lots of secondary cracks were observed. Moreover, the residual strain at the grain boundary was larger than that of the interior of grains.

316L austenitic stainless steel (SS) has excellent mechanical properties and corrosion resistance and is widely used in the primary pipeline material of PWR nuclear power plants. The reactor is generally composed of a plurality of parallel loops. The SS generator connects the steam generator and the main coolant pump in each loop to a closed loop. In the process of installation, it is unavoidable to use the SS bent pipe material. After the cold forming of the inside of the elbow, there is a cold deformation between 15% and 35%, and the cold deformation in different parts of the elbow is not uniform [1]. A large number of experimental studies [2,3] showed that cold-worked 316L SS is prone to stress corrosion cracking failure in high temperature and high pressure water, and the stress corrosion crack propagation rate increases with the degree of cold working. An intragranular stress corrosion crack was detected inside the 316LN SS elbow in a domestic nuclear power plant [1]. Long-term operating experience of nuclear power plants shows that stress corrosion cracking is the main failure mode of SS main pipeline materials, which will cause long-term and significant shutdown, repair, and even nuclear radiation leakage.
In the past 30 years, a large number of researches abroad have focused on the stress corrosion crack propagation behavior of the as-molded cast 316L SS in high-temperature and high-pressure water. The research on the cold-processed 316L SS is also mainly directed to the roll-formed sheet[2] and the actual use of nuclear power plants. The 316L SS tubing, especially the study of bends, has rarely been reported. In addition, the domestic research on SS in high temperature and high pressure water is mainly focused on its oxide film [4] and electrochemical behavior [5], etc., or the U bend specimen [6] or double cantilever beam specimen [7] The stress corrosion crack propagation behavior under extreme conditions was obtained in a static high temperature autoclave containing a high temperature alkaline solution. In recent years, the development of stress corrosion crack propagation behavior of high-temperature and high-pressure circulating water in which SS materials are used to simulate nuclear power in the field has only been studied [3,8–11].
In a refueling cycle of a pressurized water reactor nuclear power plant, the concentration of boron and lithium in the primary circuit water is very high at the initial stage of operation, and the concentration of boron lithium gradually decreases during the later period of operation and shutdown, and the boron and lithium solution will change the pH value of the solution and thus affect the stress corrosion of the material. Behavior [12]. At the same time, the temperature of the primary circuit water will change from room temperature to 325 °C during the start-up and shutdown process. The temperature can affect the crack propagation behavior by affecting the dissolution of metal ions, corrosion potential, chemical balance and crack tip oxide dissolution. [13]. In this experiment, the stress corrosion crack propagation behavior of 316LN SS elbows used in nuclear power plants in high temperature and high pressure circulating water was studied by in-situ measurement of crack lengths of compact tensile (CT) specimens by direct current potential drop (DCPD). The effect of lithium solution and different temperatures on crack growth rate. The obtained stress corrosion crack propagation data close to the actual operating conditions can provide important data support for aging management and life assessment of nuclear power plant equipment.

1 Experimental method
The experimental material was a 316LN SS elbow[1] in the main pipeline of a nuclear power plant in China. Its diameter was 355.6 mm and its wall thickness was 37~45.5 mm. See Figure 1a. The chemical composition (mass fraction, %) of the elbow was: C 0.022, Si 0.44, Mn 1.85, P 0.029, Cr 17.56, Ni 12.32, Mo 2.63, S 0.003, Cu 0.21, V 0.086, Co 0.14, Nb 0.015, N 0.08, Fe balance. The elbow was processed by cold deformation and was not treated afterwards. The stress corrosion cracking occurred during the actual service. According to the ASTM-E399 standard, a 12.5 mm thick compact (1/2T CT) specimen is taken near the crack inside the elbow so that the specimen crack propagates from the inside to the outside along the elbow (Figure 1b). The specific dimensions of the sample are shown in Figure 2. The Vickers hardness around the sample notch is about 242 HV0.5. Marin et al. [14] pointed out that the Vickers hardness of austenite SS increases with the degree of cold work. By comparison, the degree of cold processing near the notch of this experimental sample is about 17%.

20180403091646 89722 - Stress Corrosion Cracking Behavior of Nuclear Grade 316LN Stainless Steel Bend in High Temperature and Pressure Water

Fig.1 Schematic illustrations of the 316LN SS Bend (a) and the location of the 1/2T CT specimen (b)

20180403091756 76254 - Stress Corrosion Cracking Behavior of Nuclear Grade 316LN Stainless Steel Bend in High Temperature and Pressure Water

Fig.2 Dimensions of the 1/2T CT specimen

In the air at room temperature, fatigue fatigue pre-cracking experiments were performed on CT specimens using a SFL-5-350 fatigue machine to obtain a pre-crack with a length of approximately 1.5 mm. Among them, the parameters for loading the triangular wave are: the maximum stress intensity factor Kmax=15 MPam1/2, the stress ratio (minimum load/maximum load) R=0.2, and the frequency f=20 Hz. After the pre-cracking in air was completed, grooves with a depth of 5% of the sample thickness were cut along the crack propagation direction on both sides of the sample.
CT crack growth experiments were carried out in an autoclave equipped with a high-temperature, high-pressure circulating water system. The experimental setup was described in detail in [15]. The crack length of the specimen was collected in real time by the DCPD data acquisition system [3,10]. Pure water or boron-lithium solution (1500 mg/L B+2.3 mg/L Li) was used in the experiment. The boron-lithium solution was prepared from H3BO3 and LiOHH2O. The maximum oxygen content in the PWR nuclear power plant coolant should not exceed. 0.1 mg/L, and the SS material has higher stress corrosion sensitivity in the dissolved oxygen environment [16], so the dissolved oxygen concentration of the solution in the control tank of this experiment is 0.1 mg/L, and the solution pressure in the autoclave is 15.6 MPa. When the temperature reaches 310 °C and is stable for 24 h, the CT samples are first loaded with R, 0.3, 0.5, and 0.7, Kmax is 20 MPam1/2, and a triangular wave with f of 0.01 Hz is used to prefabricate corrosion fatigue cracks. It is better to promote the crack to change from the common transgranular fatigue cracking mode to the stress corrosion cracking (SCC) mode, and then to load the trapezoidal wave for the stress corrosion crack propagation experiment, where R is 0.7, Kmax is 20 MPam1/2, and the dead load time For 3 h, the loading and deloading time were 500 s.The effect of boron and lithium solution and temperature on the stress corrosion crack propagation behavior of 316LN SS pipe material was studied by changing the experimental solution and the experimental temperature (270-330 °C). The experimental parameter statistics are shown in Table 1.

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Table 1 Test conditions of the stress corrosion cracking and crack growth rates for 316LN SS in high temperature high pressure water at 270~330 ℃
After the stress corrosion experiment was finished, a 2.5 mm thick sheet specimen was cut from the side of the CT specimen for analysis of the crack propagation path. After polishing the plate specimens with sandpaper to 2000#, mechanical polishing was performed with a diamond polishing slurry with a particle size of 1.5 μm. Finally, a manual polishing was performed with a MasterMet 2SiO 2 suspension, thereby reducing the residual strain introduced on the surface of the specimen due to mechanical deformation. . The FEI XL30 environmental scanning electron microscope (SEM) equipped with an electron backscattered diffraction (EBSD) test system was used to analyze the microscopic characteristics of the grain boundary types and residual strains in the crack propagation path and its vicinity. The CT specimens were fatigued and broken in the air. The fracture morphology was analyzed using a stereomicroscope and SEM. The length of the stress corrosion crack propagation was measured several times along the crack propagation direction and the average of the measurement results was averaged to obtain the actual stress corrosion crack propagation length, which was used to calibrate the measured value of the DCPD system.
2 Results and Discussion
2.1 Corrosion fatigue crack propagation in high temperature and high pressure water
Fig. 3 is a graph of the crack length as a function of time for a 316LN SS in a pre-corrosion fatigue crack in high-temperature high-pressure water. In the same stage, the crack length and time are in a good linear relationship, which means that the cracks in the specimen are stably expanded during the corrosion fatigue stage. The slope of the curve in a certain stage can be used to obtain the corresponding crack propagation rate value. As R changes from 0.3 to 0.5 and 0.7 in order, the crack length versus time curve becomes more and more gentle, indicating that the crack growth rate is getting lower and lower. In the CF#1 stage (R=0.3), the 316LN SS crack propagation rate is 1.3×10-6 mm/s; when R increases to 0.5 (CF#2 stage), the crack propagation rate drops to 6.4×10-7 mm /s, 50.8% lower than before; when R is increased again to 0.7 (CF#3 stage), the crack growth rate is further reduced to 9.5×10-8 mm/s, which is 85.2% lower than when R is 0.5. The corrosion fatigue crack growth rate of 316LN SS in high temperature and high pressure water decreases significantly with the increase of R. The crack growth rate at R 0.3 is 13.7 times that at R 0.7. Under the other conditions unchanged, control R can reduce the corrosion crack growth rate of SS corrosion, thereby extending the service life of components [10].
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Fig.3 Crack length vs time curve of 316LN SS during corrosion fatigue in high temperature high pressure water at 310 ℃

2.2 Stress corrosion crack propagation in high temperature and high pressure water
2.2.1 Effect of Boron Lithium Solution on Crack Growth Rate After the corrosion fatigue pre-crack, the 316LN SS-loaded trapezoidal wave was subjected to stress corrosion crack propagation experiments. The results of the experimental conditions and crack growth rates at different stages were statistically shown in Table 1. The length change curve with time is shown in Figure 4. In the SCC#1 phase (310 °C), the curves are relatively flat, which indicates that the initial stage is the stress corrosion crack initiation process. At this time, the crack propagation rate is only 2.1×10-8 mm/s, which is lower than the crack growth of CF3 in corrosion fatigue stage. Rate (9.5 x 10-8 mm/s). After about 160 hours, the curve gradually became steeper and linear, indicating that the stress corrosion crack began to expand and reached a state of stable expansion. The crack growth rate is also increased first and then stabilized at 2.0×10-7 mm/s, which is 9.5 times the initial crack growth rate. The existence of crack initiation stage in the early stage of stress corrosion has also been reported in the literature [17]. The crack will gradually change from the corrosion fatigue transgranular cracking mode to the stress corrosion transgranular cracking mode. After replacing the pure water with the lithium borate solution (SCC #2), the crack growth curve did not change significantly, and the crack growth rate was 2.2×10-7 mm/s, which was basically the same as the crack growth rate in the pure water environment. Andresen et al. [18] investigated the effect of 304SS on the growth of stress corrosion cracks at 288 °C in high temperature and high pressure water, replacing pure water (pH=5.6) with 1000 mg/L B+1 mg/L Li solution (pH=6.54). After that, it shows that there is almost no change in crack propagation. The pHSC4 commercial software developed by Duke Power Company can calculate, the pH value of purified water and 1500 mg/L B+2.3 mg/L Li solution is 3.75 and 6.95 at 310 °C, respectively. In addition, Wang et al. [19] reported that when the dissolved oxygen concentration is 100 mg/L, the corrosion potential of Fe-Cr-Ni alloy in high temperature and high pressure water is about 0 V. From the Pourbaix chart [20] (Fig. 5) of the Fe-Cr-Ni alloy, the Fe-Cr-Ni alloy will generate NiFe2O4 at a dissolved oxygen concentration of 100 mg/L in 310 °C pure water (pH 5.75). Oxide film, and after replacing pure water with boron lithium solution (pH 6.95), the oxide film is still NiFe2O4, so the crack growth rate does not change significantly.
20180403092344 55824 - Stress Corrosion Cracking Behavior of Nuclear Grade 316LN Stainless Steel Bend in High Temperature and Pressure Water

Fig.4 Curve of crack length vs time for 316LN SS during stress corrosion cracking in high temperature high pressure water at 270~310 ℃

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Fig.5 Pourbaix diagram for nickel species in the ternary system of Fe-Cr-Ni at 300 ℃ and [Fe(aq)]tot=[Cr(aq)]tot=[Ni(aq)]tot=10-6 molal[20]

In the boron-lithium solution at 330 °C (SCC #5 stage), the stress corrosion crack growth rate of 316LN SS is 2.5 × 10-7 mm/s. In the SCC#6 stage, after the boron-lithium solution was replaced with pure water, the crack length curve became smoother over time (Fig. 4), and the crack growth rate was reduced to 8.6×10-8 mm/s, which was higher than that of boron lithium solution. The crack propagation rate in the steel is reduced by 65.6%. This phenomenon is similar to the results of Tice et al. [12] on cold-worked 304SS. The crack growth rate in pure water at 300 °C (pH 5.70) is higher than that in 2 mg/L Li solution (pH 7.22). The rate is 35.7% lower. At 330 °C, the pH values of pure water and 1500 mg/L B+2.3 mg/L Li were 5.90 and 7.28, respectively. According to the Pourbaix diagram (Fig. 5), the Ni in Fe-Cr-Ni alloy has a potential of about 0 V and a pH of about 7.2, which is exactly on the balance line between NiFe2O4 and NiO, while the NiO has low protection. In NiFe2O4 [21], the corrosion resistance of 316LN SS in boron-lithium solution at 330 °C is lower than that in pure water, resulting in a higher rate of stress corrosion crack propagation. In summary, the boron-lithium solution has a certain influence on the crack growth rate of SS in high-temperature and high-pressure water, and its influence degree is related to the pH of the solution at a specific temperature.
2.2.2 Effect of solution temperature on crack growth rate In SCC#2~SCC#5 stage, the effect of different solution temperature on the stress corrosion crack propagation rate of 316LN SS was studied. From Fig. 4, it can be seen that the change of temperature makes the crack length change with time, and the slope of the curve is kept constant under a certain temperature condition, which shows that the crack spreads steadily. The relationship between crack growth rate and temperature is shown in Fig. 6. The crack growth rate monotonically increases with increasing temperature. When the temperature is increased from 270 °C to 330 °C, the crack growth rate increases 1.7 times.
20180403092624 81452 - Stress Corrosion Cracking Behavior of Nuclear Grade 316LN Stainless Steel Bend in High Temperature and Pressure Water

Fig.6 Effect of temperature (270~310 ℃) on the crack growth rate of 316LN SS during SCC test

Andresen et al. [13] proposed that the stress corrosion crack propagation behavior of austenite SS in high temperature and high pressure water conformed to the slip-oxidation model. When the crack propagates, the exposed metal of the crack tip is first oxidized, the oxide film near the grain boundary is broken under the action of stress or chemical media, and then the grain boundary dissolves to advance the crack. The above process is repeated continuously. Temperature can affect crack propagation behavior by affecting metal ion dissolution, corrosion potential, chemical equilibrium, and crack tip oxide dissolution. The crack propagation of austenite SS in high-temperature high-pressure water is a heat-activated process. The apparent activation energy (Eaae) can be calculated by the following equation: E aae = R × T 1 × T 2 T 2 – T 1 × ln CG R 2 CG R 1 (1)
Among them, Eaae is the apparent activation energy, R is the molar gas constant, T1 and T2 are the absolute temperatures, and CGR1 and CGR2 are the crack growth rates of the sample under T1 and T2 temperature conditions, respectively. In the stage of SCC#2~SCC#3, the temperature decreased from 310 °C to 270 °C, the crack growth rate decreased from 2.2×10-7 mm/s to 9.1×10-8 mm/s, which was a 58.6% reduction. Using formula (1) to find the corresponding Eaae is 56.5 kJ/mol, and 30% cold-worked 316L SS obtained by Du et al. [9] is consistent with Eaae (57.3 kJ/mol) at a temperature range of 200-325°C. When the temperature was increased from 270 °C (SCC #3 stage) to 290 °C (SCC #4 stage), the crack growth rate slightly increased to 9.9 x 10-8 mm/s, and the corresponding Eaae calculation was only 11.7 kJ/mol. The experimental course of the sample in high temperature and high pressure water may affect the crack growth rate [17]. The low level of Eaae may be related to the experimental process that the temperature first rapidly decreases from high temperature (330 °C) to 270 °C and then to 290 °C. When Zhu et al. [15] studied the 316L heat affected zone, the temperature first decreased from 340 °C to 260 °C and then increased to 280 °C, but the crack growth rate slightly decreased after temperature increase. During SCC#5~SCC#6, the temperature increased from 290 °C to 330 °C, the crack growth rate increased from 9.9×10-8 mm/s to 2.5×10-7 mm/s, and the corresponding Eaae was 64 kJ. /mol, which is consistent with the stress corrosion crack propagation of Eaae (64.2 kJ/mol) of 20% cold-worked 316 SS obtained by Andresen et al. [23] in 288-340 °C hydrogen-dissolved high-temperature high-pressure water. The data of four crack propagation rates in the temperature range of 270~330 °C were fitted to the Eaae of 316LN SS elbow specimens in high temperature and high pressure water. The Eaae is 52 kJ/mol, which is similar to Du et al. [9]. ] Andresen et al. [23] have similar results for 20%~30% cold-worked 316L SS.
2.3 sample fracture observation
After the 316LN SS specimen was broken in the air, the section was observed with a stereomicroscope. The results are shown in Figure 7. The results show that the fracture morphology and color in the three stages of pre fatigue cracking in air, pre-corrosion fatigue corrosion in water, and stress corrosion cracking in water are different and can be distinguished. The section of the pre-crack stage is relatively flat, while the section of the stress corrosion crack propagation stage is relatively rough, and the front of the section corresponding to each stage is straight. Further observation of the cross-section with SEM (Fig. 8) shows that the section of the pre-crack stage in water corrosion is transgranular cracking; when the loading mode is transformed from a triangular wave to a trapezoidal wave, the crack transitions from transgranular cracking to intergranular cracking (Figure 8b). Corresponding to Fig. 4, SCC#1 has an initial stage of slow crack growth. The stress corrosion fracture presents a rock sugar-like pattern (Fig. 8c), which is a typical cracking morphology. The crack propagation length was measured multiple times (39 times) along the crack propagation direction on the stress corrosion cracking portion and finally averaged to obtain a crack extension length of 0.981 mm after 316LN SS was subjected to high temperature and high pressure water stress corrosion test for about 2047 h.
20180403092925 56367 - Stress Corrosion Cracking Behavior of Nuclear Grade 316LN Stainless Steel Bend in High Temperature and Pressure Water

Fig.7 Optical microscope image of the fracture surface of 316LN SS after stress corrosion test in high temperature high pressure water at 270~310 ℃

After polishing the flake sample removed from the CT sample, the backscattered electron image of the SEM (Fig. 9) shows that the initial crack growth path is relatively flat, corresponding to the creep mode of the corrosion fatigue phase; the crack propagation path thereafter Bifurcation occurs, cracks go forward in a zigzag manner, and there are more secondary cracks, cracking along the crystal stress corrosion. The crack propagation path analysis is consistent with the results of cross-sectional observations (Figure 8). In order to further analyze the microscopic characteristics of grain boundary distribution, grain orientation, and residual strain near the crack propagation path, EBSD analysis was performed on the sample near the crack tip (Fig. 10a). The curves of different colors in Fig. 10b represent different grain boundaries, in which the green curve represents the 5°~15° low angle grain boundary, the blue curve represents the 15°~180° high angle grain boundary, and the red curve represents the coincident position lattice (CSL). ) Grain boundaries. As can be seen from the analysis of Figures 10a and b, the crack propagates only along the high-angle grain boundary and no cracks are seen at the grain boundary of the CSL. Because high-angle grain boundaries have higher energy, CSL grain boundaries are ordered low-energy grain boundaries and have excellent resistance to intergranular stress corrosion [24]. The core average orientation difference (KAM) is the average value of the orientation difference between a certain point and its neighbors within the grain. The larger the KAM value, the greater the residual strain at the corresponding position inside the material. In the KAM diagram (Fig. 10c), there are more blue crystals in the grains, and the green and yellow grains at the grain boundaries are more concentrated, indicating that the KAM value inside the grains is lower than the KAM value at the grain boundaries, so the residual strain at grain boundaries is greater than that of crystals. Residual strain inside the grain. The occurrence of intergranular stress corrosion cracking in high temperature and high pressure water in 316LN SS is related to the existence of high residual strain at grain boundaries.

20180403093058 65105 - Stress Corrosion Cracking Behavior of Nuclear Grade 316LN Stainless Steel Bend in High Temperature and Pressure Water

Fig.8 SEM images of the fracture surface of 316LN SS tested in high temperature high pressure water at 270~310 ℃: (a) overall morphology; (b) initial morphology, showing the transformation from transgranular fatigue corrosion crack to intergranular stress corrosion crack; (c) typical intergranular stress corrosion crack

20180403093159 50038 - Stress Corrosion Cracking Behavior of Nuclear Grade 316LN Stainless Steel Bend in High Temperature and Pressure Water

Fig.9 SEM image of the crack path of 316LN SS after stress corrosion test in high temperature high pressure water at 270~310 ℃

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Fig.10 EBSD images of the crack paths of 316LN SS after stress corrosion test in high temperature high pressure water at 270~310 ℃: (a) SEM morphology, (b) grain boundary characters, (c) inverse pole figure, (d) Kernel average misorientation

3 Conclusion
(1) The 316LN SS elbow has high stress corrosion sensitivity in high temperature and high pressure water.
(2) The stress corrosion crack growth rate of 316LN SS in high temperature and high pressure water increases monotonically with the increase of temperature; the crack propagation Eaae in the temperature range of 270~330 °C is 52 kJ/mol.
(3) Boron-lithium solution has a certain influence on the crack growth rate of 316LN SS in high-temperature and high-pressure water, and the degree of influence is related to the pH of the solution at a specific temperature.
(4) The stress corrosion fracture is a typical crack initiation morphology, and the crack propagation path only follows the high-angle grain boundary and does not follow the CSL grain boundary, and a large number of secondary cracks are observed at the same time.
The authors have declared that no competing interests exist.

Source: Network Arrangement – China Stainless Steel Bend Manufacturer – Yaang Pipe Industry (www.metallicsteel.com)

(Yaang Pipe Industry is a leading manufacturer and supplier of nickel alloy and stainless steel products, including Super Duplex Stainless Steel Flanges, Stainless Steel Flanges, Stainless Steel Pipe Fittings, Stainless Steel Pipe. Yaang products are widely used in Shipbuilding, Nuclear power, Marine engineering, Petroleum, Chemical, Mining, Sewage treatment, Natural gas and Pressure vessels and other industries.)

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