Effect of SO42− concentration on corrosion damage of 304 stainless steel in Cl− solution
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摘要: 为了研究SO42−对含有0.7 mol/L Cl−溶液中304不锈钢腐蚀损伤的影响，采用声发射技术与形貌观察技术分别测试试样腐蚀过程中产生的声信号和腐蚀前后试样表面形貌。结果表明：在Cl−/SO42−溶液中，随着SO42−浓度的增加，304不锈钢腐蚀过程产生的AE信号相对能量与幅度较大值、撞击累积数曲线斜率、持续时间等参数先减小后增加；腐蚀坑与龟裂块状的腐蚀产物数量先减少后增加，由龟裂腐蚀产物引起的表面疏松程度先紧密后疏松。试样腐蚀损伤发生的时间因SO42−离子浓度不同，0、0.10、0.25和0.40 mol/L时试样损伤发生的时间段分别为腐蚀的前中期、前期、后期以及全程时间段。腐蚀损伤程度由强到弱的顺序为0 mol/L> 0.40 mol/L> 0.10 mol/L > 0.25 mol/L。综合试样腐蚀形貌与声发射参数，在本试验范围内，对于含0.7 mol/L Cl−溶液中，为了减轻304不锈钢腐蚀发生，添加SO42−离子的适宜浓度为0.25 mol/L。Abstract: In order to investigate the effect of SO42− on the corrosion damage of 304 stainless steel in a solution containing 0.7 mol/L Cl−, acoustic emission technology and morphology observation technology were used to test the acoustic signal generated during the corrosion process and the surface morphology of the sample before and after corrosion, respectively. In the Cl−/SO42− solution, with the increase of SO42− concentration, the parameters such as relative energy and amplitude of AE signal generated during the corrosion process, the slope of cumulative number of impacts and duration time, as well as the number of corrosion pits and the number of cracked massive corrosion products firstly decrease and then increase. The degree of surface looseness caused by cracked corrosion products is firstly tight and then loose with the increase of SO42− concentration. The time period of sample corrosion damage is different due to the concentration of SO42− ions. The time periods for sample damage at 0, 0.10, 0.25, and 0.40 mol/L concentrations are the early and mid-term, early, late and full time periods of corrosion, respectively. The order of SO42− ion concentration influencing the degree of corrosion damage from heavy to light is 0 mol/L> 0.40 mol/L> 0.10 mol/L> 0.25 mol/L. In this study, after evaluating sample corrosion morphology and acoustic emission parameters, appropriate concentration of SO42− ions of 0.25 mol/L can effectively reduce the corrosion of 304 stainless steel in a 0.7 mol/L Cl− solution.
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图 1 304不锈钢点腐蚀试验装置示意
Figure 1. Schematic diagram of spot corrosion test device used in this study
图 2 冷加工的304不锈钢光学显微组织
Figure 2. Optical microstructure of as-cold working 304 stainless steel
图 3 不同SO42−浓度下304不锈钢腐蚀试验过程中AE相对能量随时间的变化
Figure 3. Change of AE relative energy with time during corrosion test of 304 stainless steel under different SO42− concentration
(a) 0 mol/L；(b) 0.1 mol/L；(c) 0.25 mol/L；(d) 0.40 mol/L
图 4 不同SO42−浓度下AE幅度和撞击累积数随时间变化
Figure 4. Changes of AE amplitude and cumulative number of impacts with time under different SO42− concentrations
(a) 0 mol/L；(b) 0.1 mol/L；(c) 0.25 mol/L；(d) 0.40 mol/L
图 5 AE信号持续时间-幅度-腐蚀时间关系
Figure 5. Relationship between AE signal duration and amplitude-time
(a) 0 mol/L；(b) 0.1 mol/L；(c) 0.25 mol/L；(d) 0.40 mol/L
图 6 腐蚀前后试样表面形貌
(a)腐蚀前；(b) 0 mol/L；(c) 0.1 mol/L；(d) 0.25 mol/L；(e) 0.40 mol/L
Figure 6. Morphologies of the sample surface before and after corrosion
图 7 腐蚀后试样表面的SEM形貌
Figure 7. SEM morphologies of the sample surface after corrosion
(a) 0 mol/L；(b) 0.1 mol/L；(c) 0.25 mol/L；(d) 0.40 mol/L
表 1 试样腐蚀过程中声发射信号数量及占比
Table 1. The number and proportion of acoustic emission signals during sample corrosion
SO42− 浓度/（mol·L−1） 腐蚀时间/s AE 信号撞击积累数/个 AE 信号幅度/dB 信号相对能量占比/% < 2 2～10 >10 0 0～1800 15123 4794 99.833 0.125 0.042 1800～3600 5529 99.910 0.054 0.036 3600～5400 4800 99.958 0.042 0.1 0～1800 3015 1307 99.617 0.077 0.306 1800～3600 877 99.886 0.114 3600～5400 831 100.000 0.25 0～1800 11857 3008 100.000 1800～3600 4058 100.000 3600～5400 4791 99.979 0.021 0.40 0～1800 6959 2253 99.112 0.666 0.222 1800～3600 2130 99.718 0.235 0.047 3600～5400 2576 99.922 0.078 
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表 2 试样的AE信号幅度值和持续时间占比
Table 2. Proportion of AE signal amplitude and duration of the sample
SO42− 浓度/
(mol·L−1)腐蚀时间/s 信号幅度值占比 /% 持续时间占比 /% <30 dB 30～40 dB >40 dB <100 μs >100 μs 0 0～1800 99.708 0.271 0.021 99.791 0.209 1800～3600 99.910 0.054 0.036 99.801 0.199 3600～5400 99.979 0.021 99.896 0.104 0.10 0～1800 98.746 0.868 0.386 99.614 0.386 1800～3600 99.890 0.110 100.000 3600～5400 100.000 100.000 0.25 0～1800 100.000 99.100 0.100 1800～3600 100.000 99.877 0.123 3600～5400 99.958 0.042 99.937 0.063 0.40 0～1800 98.935 0.799 0.266 99.068 0.932 1800～3600 99.596 0.314 0.090 99.624 0.376 3600～5400 99.884 0.116 99.845 0.155
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