基于<strong>PDM</strong>的<strong>304</strong>不锈钢钝化膜生长动力学研究

doi:10.11902/1005.4537.2022.269

中国腐蚀与防护学报

2023, Vol. 43

Issue (4): 911-921 CSTR: 32134.14.1005.4537.2022.269 DOI: 10.11902/1005.4537.2022.269

研究报告

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基于PDM的304不锈钢钝化膜生长动力学研究

毛飞雄¹(

), 周羽婷², 姚文清², 沈翔³, 肖龙³, 李明辉³

^1.中国科学院宁波材料技术与工程研究所中国科学院海洋新材料与应用技术重点实验室浙江省海洋材料与防护技术重点实验室宁波 315201
^2.东北大学冶金学院沈阳 110819
^3.宁波市杭州湾大桥发展有限公司宁波 315201

Growth Kinetics of Steady-state Passive Film on Type 304 Stainless Steel Based on Point Defect Model

MAO Feixiong¹(

), ZHOU Yuting², YAO Wenqing², SHEN Xiang³, XIAO Long³, LI Minghui³

^1.Key Laboratory of Marine Materials and Related Technologies, Zhejiang Key Laboratory of Marine Materials and Protective Technologies, Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201, China
^2.School of Metallurgy, Northeastern University, Shenyang 110819, China
^3.Ningbo Hangzhou Bay Bridge Development Co. LTD, Ningbo 315201, China

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摘要:

研究了304不锈钢在不同pH溶液中钝化膜生长规律。结果表明，304不锈钢表面生长的钝化膜为n型半导体，钝化膜内施主密度与施加的电位成反比 (除pH=13.4溶液)；在钝化区内，稳态电流密度与施加的电位无关，而阻挡层的厚度随施加电位增加而增厚。采用点缺陷模型 (PDM) 对钝化区的电化学阻抗谱 (EIS) 数据进行分析计算，拟合出的参数可以用来预测样品随时间的腐蚀进程。计算结果表明，间隙阳离子是阻挡层的主要缺陷，缺陷的扩散系数约为10^-19 cm²·s^-1。

关键词 ： 304不锈钢, 钝化, 点缺陷模型, 电化学阻抗谱

Abstract：

The passivity of type 304 stainless steel in aqueous solution at different pH values has been assessed, and the acquired data suggest that the passive ﬁlm formed on type 304 SS is n-type semiconducting, and the donor density within the passive film is inversely proportional to the applied voltage except those in pH=13.4 solution. The current density in steady-state is voltage-independent in the passive range, while the thickness of the barrier layer has a linear relationship with the applied voltage, which are satisfied with the statements of the point defect model (PDM). EIS data are analyzed with the PDM by optimizing the model on the data using genetic algorithm approach. In addition, the impedance data over the entire passive range can be described by the fitted parameters, which can be utilized to predict the corrosion evolution of the sample as a function of time. The results of the optimization indicate that interstitial cations are the dominant defects in the barrier layer and that the diffusivity of the defect is about 10^-19 cm²·s^-1.

Key words： 304 stainless steel passivity point defect model EIS

收稿日期: 2022-08-31 32134.14.1005.4537.2022.269

ZTFLH:

TG174

基金资助:宁波市重点研发计划(2021Z079);中科院国际合作伙伴项目(174433KYSB20200006)

通讯作者: 毛飞雄，E-mail: maofeixiong@nimte.ac.cn，研究方向为海洋腐蚀与防护

Corresponding author: MAO Feixiong, E-mail: maofeixiong@nimte.ac.cn

作者简介: 毛飞雄，男，1986年生，副研究员

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引用本文:

毛飞雄, 周羽婷, 姚文清, 沈翔, 肖龙, 李明辉. 基于PDM的304不锈钢钝化膜生长动力学研究[J]. 中国腐蚀与防护学报, 2023, 43(4): 911-921.
MAO Feixiong, ZHOU Yuting, YAO Wenqing, SHEN Xiang, XIAO Long, LI Minghui. Growth Kinetics of Steady-state Passive Film on Type 304 Stainless Steel Based on Point Defect Model. Journal of Chinese Society for Corrosion and protection, 2023, 43(4): 911-921.

链接本文:

https://www.jcscp.org/CN/10.11902/1005.4537.2022.269 或 https://www.jcscp.org/CN/Y2023/V43/I4/911

图1 PDM中假设的表示点缺陷产生和湮灭的界面反应

Reaction	$a i / V - 1$	$b i / c m - 1$	c_i	Units of $k i 0$
(1) $m + V M χ' → k 1 M M + ν m + χ e'$	$α 1 (1 - α) χ γ$	$- α 1 χ K$	-α₁βχγ	$1 S$
(2) $m → k 2 M i χ + + ν m + χ e'$	$α 2 (1 - α) χ γ$	$- α 2 χ K$	-α₂βχγ	$m o l c m 2 ⋅ s$
(3) $m → k 3 M M + χ 2 V O ∙ ∙ + χ e'$	$α 3 (1 - α) χ γ$	$- α 3 χ K$	-α₃βχγ	$m o l c m 2 ⋅ s$
(4) $M M → k 4 M δ + + (δ - χ) e'$	$α 4 α δ γ$	-	α₄βδγ	$m o l c m 2 ⋅ s$
(5) $M i χ + → k 5 M δ + + (δ - χ) e'$	$α 5 α δ γ$	-	α₅βδγ	$c m s$
(6) $V O ∙ ∙ + H 2 O → k 6 O O + 2 H +$	$2 α 6 α γ$	-	α₆βδγ	$c m s$
(7) $M O χ / 2 + χ H + → k 7 M δ + + χ 2 H 2 O + (δ - χ) e'$	$α 7 α (δ - χ) γ$	-	α₇(δ-χ)βγ	$m o l c m 2 ⋅ s$

表1 界面反应的速率常数表达式ki=ki0eaiVebiLecipH中的系数

图2 304不锈钢在不同溶液中的动电位极化曲线

图3 304不锈钢在不同溶液中的稳态 (恒电位极化) 电流密度与电位及电流随时间的曲线

图4 304不锈钢在不同pH溶液中施加不同恒电位极化6 h后的Mott-Schottky曲线和阻挡层的施主密度

图5 304不锈钢在pH=1.4溶液中0.5 VSCE恒电位极化后的EIS和K-K变换曲线

图6 拟合阻抗数据的等效电路图

图7 304不锈钢在不同溶液中施加不同电位极化后的EIS图

Parameter	0.3 / V	0.4 / V	0.5 / V	Stage optinization
Polarizability α	0.45	0.45	0.44	Second stage optimization
Transfer coeff. α₂	0.23	0.23	0.23	Average of first stage optimization
Transfer coeff. α₃	0.66	0.66	0.66	Average of first stage optimization
Transfer coeff. α₇	0.49	0.49	0.49	Average of first stage optimization
Rate constant $k 200 /$ mol·cm^-2·s^-1	4.67×10^-13	4.67×10^-13	4.67×10^-13	Average of first stage optimization
Rate constant $k 300$ / mol·cm^-2·s^-1	3.78×10^-17	3.78×10^-17	3.78×10^-17	Average of first stage optimization
Rate constant $k 700$ / mol·cm^-2·s^-1	6.16×10^-15	6.16×10^-15	6.16×10^-15	Average of first stage optimization
CPE-Y / S·s ^α ·cm^-2	4.18×10^-5	3.92×10^-5	3.86×10^-5	Second stage optimization
CPE-α	0.94	0.95	0.95	Second stage optimization
Warburg coeff. σ / Ω·cm²·s^-0.5	3.03×10⁵	2.14×10⁵	1.56×10⁵	Second stage optimization
Electronic resistance R_{e, h} / Ω·cm²	7.82×10⁶	1.72×10⁷	9.93×10¹²	Second stage optimization
Double layer capacitance C_dl / F·cm^-2	1.51×10^-4	9.56×10^-5	6.91×10^-5	Second stage optimization
Charge transfer resistance R_ct / Ω·cm²	1.75×10⁵	2.88×10⁵	4.22×10^-5	Second stage optimization
Strength of electric field ε / V·cm^-1	2.03×10⁶	2.03×10⁶	2.03×10⁶	Average of first stage optimization
Kinetic order of H⁺n	0.5	0.5	0.5	Average of first stage optimization
Current density I_ss / nA·cm^-2	16.15	20.24	24.56	Second stage optimization
Thickness of barrier layer L_ss / nm	1.24	1.47	1.74	Second stage optimization
Diffusivity of principal defect D / cm²·s^-1	1.34×10^-18	8.64×10^-19	6.43×10^-19	Second stage optimization

表2 304不锈钢在pH=1.4溶液中不同钝化膜形成电位下PDM最优化模型参数值

Parameter	0.3 / V	0.4 / V	0.5 / V	Stage optinization
Polarizability α	0.34	0.25	0.25	Second stage optimization
Transfer coeff. α₂	0.23	0.23	0.23	Average of first stage optimization
Transfer coeff. α₃	0.66	0.66	0.66	Average of first stage optimization
Transfer coeff. α₇	0.49	0.49	0.49	Average of first stage optimization
Rate constant $k 200$ / mol·cm^-2·s^-1	4.67×10^-13	4.67×10^-13	4.67×10^-13	Average of first stage optimization
Rate constant $k 300$ / mol·cm^-2·s^-1	3.78×10^-17	3.78×10^-17	3.78×10^-17	Average of first stage optimization
Rate constant $k 700$ / mol·cm^-2·s^-1	6.16×10^-15	6.16×10^-15	6.16×10^-15	Average of first stage optimization
CPE-Y / S·s ^α ·cm^-2	7.34×10^-5	3.53×10^-5	4.14×10^-5	Second stage optimization
CPE-α	1	1	0.94	Second stage optimization
Warburg coeff. σ / Ω·cm²·s^-0.5	1.07×10⁴	6.91×10⁴	7.38×10⁴	Second stage optimization
Electronic resistance R_{e, h} / Ω·cm²	3.78×10¹²	7.07×10¹²	7.67×10¹²	Second stage optimization
Double layer capacitance C_dl / F·cm^-2	3.14×10^-5	6.99×10^-5	1.13×10^-4	Second stage optimization
Charge transfer resistance R_ct / Ω·cm²	1.08×10⁶	3.37×10⁵	4.19×10⁵	Second stage optimization
Strength of electric field ε / V·cm^-1	2.03×10⁶	2.03×10⁶	2.03×10⁶	Average of first stage optimization
Kinetic order of H⁺n	0.5	0.5	0.5	Average of first stage optimization
Current density I_ss / nA·cm^-2	15.22	13.4	15.66	Second stage optimization
Thickness of barrier layer L_ss / nm	2.36	2.99	3.33	Second stage optimization
Diffusivity of principal defect D / cm²·s^-1	1.85×10^-10	5.45×10^-19	4.66×10^-19	Second stage optimization

表3 304不锈钢在pH=5.4溶液中不同钝化膜形成电位下PDM最优化模型参数值

Parameter	0 / V	-0.1 / V	-0.2 / V	Stage optinization
Polarizability α	0.45	0.282624	0.289249	Second stage optimization
Transfer coeff. α₂	0.23	0.23	0.23	Average of first stage optimization
Transfer coeff. α₃	0.66	0.66	0.66	Average of first stage optimization
Transfer coeff. α₇	0.49	0.49	0.49	Average of first stage optimization
Rate constant $k 200$ / mol·cm^-2·s^-1	4.67×10^-13	4.67×10^-13	4.67×10^-13	Average of first stage optimization
Rate constant $k 300$ / mol·cm^-2·s^-1	3.78×10^-17	3.78×10^-17	3.78×10^-17	Average of first stage optimization
Rate constant $k 700$ / mol·cm^-2·s^-1	6.16×10^-15	6.16×10^-15	6.16×10^-15	Average of first stage optimization
CPE-Y (S·s ^α ·cm^-2	2.39×10^-5	2.70×10^-5	3.97×10^-5	Second stage optimization
CPE-α	0.91	0.91	0.89	Second stage optimization
Warburg coeff. σ / Ω·cm²·s^-0.5	8.48×10⁵	3.82×10⁵	6.28×10⁵	Second stage optimization
Electronic resistance R_{e, h} / Ω·cm²	1.00×10¹³	9.81×10¹²	9.99×10¹²	Second stage optimization
Double layer capacitance C_dl / F·cm^-2	2.23×10^-4	48.99×10^-4	2.32×10^-4	Second stage optimization
Charge transfer resistance R_ct / Ω·cm²	1.18×10⁵	2.03×10⁴	6.02×10⁴	Second stage optimization
Strength of electric field ε / V·cm^-1	2.03×10⁶	2.03×10⁶	2.03×10⁶	Average of first stage optimization
Kinetic order of H⁺n	0.5	0.5	0.5	Average of first stage optimization
Current density I_ss / nA·cm^-2	13.93	9.91	8.62	Second stage optimization
Thickness of barrier layer L_ss / nm	2.08	1.99	1.66	Second stage optimization
Diffusivity of principal defect D / cm²·s^-1	2.32×10^-18	1.08×10^-18	1.34×10^-18	Second stage optimization

表4 304不锈钢在pH=9.4溶液中不同钝化膜形成电位下PDM最优化模型参数值

Parameter	-0.2 / V	-0.3 / V	-0.4 / V	Stage optinization
Polarizability α	0.394221	0.449973	0.45	Second stage optimization
Transfer coeff. α₂	0.23	0.23	0.23	Average of first stage optimization
Transfer coeff. α₃	0.66	0.66	0.66	Average of first stage optimization
Transfer coeff. α₇	0.49	0.49	0.49	Average of first stage optimization
Rate constant $k 200$ / mol·cm^-2·s^-1	4.67×10^-13	4.67×10^-13	4.67×10^-13	Average of first stage optimization
Rate constant $k 300$ / mol·cm^-2·s^-1	3.78×10^-17	3.78×10^-17	3.78×10^-17	Average of first stage optimization
Rate constant $k 700$ / mol·cm^-2·s^-1	6.16×10^-15	6.16×10^-15	6.16×10^-15	Average of first stage optimization
CPE-Y / S·s ^α ·cm^-2	4.08×10^-5	3.65×10^-5	3.97×10^-5	Second stage optimization
CPE-α	0.88	0.92	0.92	Second stage optimization
Warburg coeff. σ / Ω·cm²·s^-0.5	3.99×10⁵	2.52×10⁵	2.26×10⁵	Second stage optimization
Electronic resistance R_{e, h} / Ω·cm²	8.28×10¹²	8.28×10¹²	7.42×10¹²	Second stage optimization
Double layer capacitance C_dl / F·cm^-2	1.35×10^-4	1.54×10^-4	2.04×10^-4	Second stage optimization
Charge transfer resistance R_ct / Ω·cm²	2.25×10⁵	1.83×10⁵	1.24×10⁵	Second stage optimization
Strength of electric field ε / V·cm^-1	2.03×10⁶	2.03×10⁶	2.03×10⁶	Average of first stage optimization
Kinetic order of H⁺n	0.5	0.5	0.5	Average of first stage optimization
Current density I_ss / nA·cm^-2	1.15	0.93	0.74	Second stage optimization
Thickness of barrier layer L_ss / nm	2.39	2.15	1.93	Second stage optimization
Diffusivity of principal defect D / cm²·s^-1	5.21×10^-18	1.54×10^-18	7.30×10^-19	Second stage optimization

表5 304不锈钢在pH=13.4溶液中不同钝化膜形成电位下PDM最优化模型参数值

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