Mn2+ 对304L和C25不锈钢在高温硝酸中腐蚀行为的协同作用机制与响应曲面模型研究

doi:10.11902/1005.4537.2025.292

中国腐蚀与防护学报

2026, Vol. 46

Issue (4): 1015-1030 CSTR: 32134.14.1005.4537.2025.292 DOI: 10.11902/1005.4537.2025.292

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Mn²⁺ 对304L和C25不锈钢在高温硝酸中腐蚀行为的协同作用机制与响应曲面模型研究

孙欣¹^,², 屈佳伟³, 高子淋³, 郑越³, 马爱利²(

), 姚琳³(

), 张连民², 郑玉贵²

^1.东北大学材料科学与工程学院沈阳 110819
^2.中国科学院金属研究所中国科学院核用材料与安全评价重点实验室沈阳 110016
^3.中国核电工程有限公司北京 100840

Mechanism and Response Surface Model for Effect of Mn²⁺ on 304L and C25 Stainless Steels in High-temperature Nitric Acid

SUN Xin¹^,², QU Jiawei³, GAO Zilin³, ZHENG Yue³, MA Aili²(

), YAO Lin³(

), ZHANG Lianmin², ZHENG Yugui²

^1.School of Materials Science and Engineering, Northeastern University, Shenyang 110819, China
^2.CAS Key Laboratory of Nuclear Materials and Safety Assessment, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China
^3.CNNC China Nuclear Power Engineering Co. Ltd., Beijing 100840, China

引用本文:

孙欣, 屈佳伟, 高子淋, 郑越, 马爱利, 姚琳, 张连民, 郑玉贵. Mn²⁺ 对304L和C25不锈钢在高温硝酸中腐蚀行为的协同作用机制与响应曲面模型研究[J]. 中国腐蚀与防护学报, 2026, 46(4): 1015-1030.
Xin SUN, Jiawei QU, Zilin GAO, Yue ZHENG, Aili MA, Lin YAO, Lianmin ZHANG, Yugui ZHENG. Mechanism and Response Surface Model for Effect of Mn²⁺ on 304L and C25 Stainless Steels in High-temperature Nitric Acid[J]. Journal of Chinese Society for Corrosion and protection, 2026, 46(4): 1015-1030.

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摘要:

核乏燃料后处理设备长期暴露于高温浓硝酸环境，且过程中产生的Mn²⁺可能影响关键不锈钢结构材料的腐蚀行为。本文系统研究了温度(60 ℃至沸腾)、硝酸浓度(3~6 mol/L)及Mn²⁺浓度(0.1~10 g/L)三因素及其交互作用对304L和C25两种奥氏体不锈钢腐蚀行为的影响。通过电化学测试、浸泡实验、扫描电镜(SEM)和X射线光电子能谱(XPS)分析，并结合响应曲面法(RSM)建立预测模型。结果表明，温度与硝酸浓度是控制腐蚀行为的最主导因素，其升高显著加速阴极反应，导致腐蚀电流密度(I_corr)增大、极化电阻(R_p)降低；Mn²⁺离子作为次要促进因素，主要通过削弱钝化膜稳定性(尤其在中低酸度环境下)加剧腐蚀。XPS分析表明，高浓度Mn²⁺会导致304L不锈钢表面Fe含量降低、Cr氧化物富集。材料对比显示，C25不锈钢因更高的Cr、Ni含量及更低的杂质元素，在所有条件下均表现出优于304L不锈钢的耐蚀性。RSM模型成功量化了各因素及其交互作用的影响，确认影响显著性顺序为：温度>硝酸浓度≫ Mn²⁺浓度。本研究为后处理设备的选材优化与工艺参数安全窗口的确定提供了重要理论依据和数据支撑。

关键词 ：不锈钢, 硝酸, Mn²⁺, 腐蚀速率, 极化电阻, 晶间腐蚀, 响应曲面法

Abstract：

Spent nuclear fuel reprocessing equipment is exposed to high-temperature concentrated nitric acid for extended durations, and the Mn²⁺ ions produced during the process may affect the corrosion behavior of key stainless steel structural materials. Herein, the effect of three factors, namely temperature (60 ℃ to boiling point), nitric acid concentration (3-6 mol/L), and Mn²⁺ ion concentration (0.1-10 g/L) of high-temperature concentrated nitric acid solutions, and their interactions on the corrosion behavior of 304L and C25 austenitic stainless steels was investigated via immersion test, electrochemical measurement, scanning electron microscopy (SEM), and X-ray photoelectron spectroscopy (XPS) analysis while a predictive model was established based on response surface methodology (RSM). The results show that temperature and nitric acid concentration are the dominant factors governing corrosion behavior, and their increase significantly accelerates the cathodic reaction, leading to an increase in corrosion current density (I_corr) and a decrease in polarization resistance (R_p). Mn²⁺ ions act as a secondary promoting factor, mainly by weakening the stability of the passive film (especially in medium and low acidity environments), thereby intensifying the corrosion. XPS analysis reveals that high concentrations of Mn²⁺ lead to a decrease in Fe content and enrichment of Cr oxides on the surface of 304L stainless steel. By comparing the corrosion characteristics of the two steels, it can be concluded that C25 stainless steel has better corrosion resistance than 304L in all conditions, these may be ascribed to higher Cr and Ni content and lower impurities for the C25 stainless steel. The RSM model successfully quantified the effect of each individual factor and their interactions and confirmed the order of the influence intensity of each factor as: temperature > nitric acid concentration ≫ Mn²⁺ concentration. The findings may provide a significant reference for the material selection and the determination of the safety window of process parameters for reprocessing equipment.

Key words： stainless steel nitric acid Mn²⁺ ions corrosion rate polarization resistance intergranular corrosion response surface method

收稿日期: 2025-09-16 32134.14.1005.4537.2025.292

ZTFLH:

TG174

基金资助:国家自然科学基金(52373321);中国科学院金属研究所创新基金(2023-PY03);中核集团领创科研项目(CNNC-LCKY-202274)

通讯作者: 马爱利，E-mail：alma@imr.ac.cn，研究方向为乏燃料后处理用材料腐蚀机理及耐蚀性设计；
姚琳，E-mail：yaolin@cnpe.cc，研究方向为乏燃料贮运及后处理设备设计和制造技术

Corresponding author: MA Aili, E-mail: alma@imr.ac.cn;
YAO Lin, E-mail: yaolin@cnpe.cc

作者简介: 孙欣，男，2001年生，硕士生

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表1 C25和304L不锈钢的化学成分 (mass fraction / %)

图1 C25和304L不锈钢的金相组织

图2 电化学测试样品的结构示意图[18]

图3 C25和304L不锈钢在含有不同浓度Mn2+、不同温度的3 mol/L和6 mol/L硝酸溶液中的开路电位(OCP)测试结果

图4 C25和304L不锈钢在含有不同浓度Mn2+、不同温度的3和6 mol/L硝酸溶液中的动电位极化曲线

	Temperature/ ℃	Nitric acid concentration / mol·L^-1	Mn²⁺ ion concentration / g·L^-1	E_{cror, SCE} / mV	I_corr/ μA·cm^-2	R_s/ Ω·cm²	CPE/ Ω^-1 s^-ⁿ cm^-2	n	R_f/ Ω·cm²	χ^-2	C_ef / F·cm^-2
C25	80	6	0.1	838.0	11.14	0.32	9.71 × 10^-5	0.93	7394	7.00 × 10^-3	6.68 × 10^-5
			1	835.4	9.20	0.47	8.32 × 10^-5	0.93	9327	8.10 × 10^-3	7.09 × 10^-5
			5	834.4	15.74	0.35	1.05 × 10^-4	0.92	7137	2.96 × 10^-3	7.39 × 10^-5
			10	848.9	15.13	0.35	1.19 × 10^-4	0.91	5972	9.60 × 10^-3	8.12 × 10^-5
	Boiling	3	0.1	582.7	0.76	0.36	3.19 × 10^-5	0.97	42500	7.96 × 10^-3	3.21 × 10^-5
			1	713.7	1.19	0.36	5.82 × 10^-5	0.96	17740	3.05 × 10^-3	5.83 × 10^-5
			5	715.8	0.99	0.40	6.20 × 10^-5	0.96	18130	6.53 × 10^-3	6.23 × 10^-5
			10	782.7	4.92	0.42	7.68 × 10^-5	0.95	9208	8.09 × 10^-3	7.53 × 10^-5
		6	0.1	879.2	58.22	0.30	1.74 × 10^-4	0.90	2059	9.14 × 10^-3	1.55 × 10^-4
			1	880.6	55.60	0.29	1.77 × 10^-4	0.90	1931	9.07 × 10^-3	1.56 × 10^-4
			5	880.3	50.47	0.30	1.75 × 10^-4	0.89	1915	8.72 × 10^-3	1.53 × 10^-4
			10	887.6	84.67	0.33	2.16 × 10^-4	0.89	1535	7.76 × 10^-3	1.87 × 10^-4
304L	60	3	0.1	513.0	0.53	0.44	4.21 × 10^-5	0.96	59540	5.56 × 10^-3	4.39 × 10^-5
			1	631.8	0.86	0.74	6.00 × 10^-5	0.95	48660	6.39 × 10^-4	6.34 × 10^-5
			5	617.4	1.11	0.41	7.21 × 10^-5	0.95	36170	4.27 × 10^-3	7.57 × 10^-5
			10	625.8	1.14	0.41	6.97 × 10^-5	0.95	29510	5.82 × 10^-3	7.21 × 10^-5
		6	0.1	791.8	3.23	0.35	6.30 × 10^-5	0.95	17250	7.87 × 10^-3	6.32 × 10^-5
			1	793.3	3.61	0.39	7.28 × 10^-5	0.95	15200	6.96 × 10^-3	7.32 × 10^-5
			5	791.1	4.54	0.44	7.09 × 10^-5	0.95	14070	8.00 × 10^-3	7.09 × 10^-5
			10	794.9	3.81	0.47	7.17 × 10^-5	0.94	14240	7.04 × 10^-3	7.18 × 10^-5
	80	3	0.1	705.4	1.34	0.69	7.42 × 10^-5	0.94	29570	1.14 × 10^-3	7.78 × 10^-5
			1	575.4	0.98	0.41	5.86 × 10^-5	0.96	30190	3.61 × 10^-3	6.02 × 10^-5
			5	563.8	1.09	0.41	6.25 × 10^-5	0.96	24800	4.95 × 10^-3	6.37 × 10^-5
			10	668.6	1.69	0.37	6.75 × 10^-5	0.96	20790	6.60 × 10^-3	6.86 × 10^-5
		6	0.1	834.8	14.18	0.33	8.69 × 10^-5	0.93	5485	9.15 × 10^-3	8.25 × 10^-5
			1	852.7	14.62	0.31	1.02 × 10^-4	0.92	4815	7.44 × 10^-3	9.53 × 10^-5
			5	851.8	14.52	0.32	1.14 × 10^-4	0.91	5205	3.46 × 10^-3	1.08 × 10^-4
			10	837.9	12.96	0.34	1.03 × 10^-4	0.93	4669	7.99 × 10^-3	9.74 × 10^-5
	Boiling	3	0.1	668.9	3.07	0.36	5.79 × 10^-5	0.96	11340	6.33 × 10^-3	5.69 × 10^-5
			1	653.9	2.80	0.39	5.89 × 10^-5	0.96	10270	6.61 × 10^-3	5.77 × 10^-5
			5	714.1	2.44	0.41	5.90 × 10^-5	0.95	12060	5.93 × 10^-3	5.80 × 10^-5
			10	709.8	3.33	0.39	6.06 × 10^-5	0.96	9674	1.56 × 10^-3	5.91 × 10^-5
		6	0.1	876.6	78.88	0.28	1.38 × 10^-4	0.92	1236	9.36 × 10^-3	1.17 × 10^-4
			1	879.1	91.72	0.39	1.48 × 10^-4	0.91	1256	1.29 × 10^-3	1.25 × 10^-4
			5	875.4	79.29	0.76	1.67 × 10^-4	0.90	1177	9.89 × 10^-3	1.41 × 10^-4
			10	881.0	91.41	0.31	1.62 × 10^-4	0.91	1159	7.99 × 10^-3	1.36 × 10^-4

表2 C25和304L在含不同浓度Mn2+离子、不同温度的3 mol/L及6 mol/L硝酸溶液中的动电位极化曲线及EIS拟合结果

图5 C25和304L不锈钢在含不同浓度Mn2+、不同温度的3 mol/L和6 mol/L硝酸溶液中的电化学阻抗谱

图6 电化学阻抗分析的等效电路[18]

图7 C25和304L不锈钢在含有不同浓度Mn2+的沸腾6 mol/L硝酸溶液中浸泡96 h后的腐蚀速率

图8 C25和304L不锈钢在含有不同浓度Mn2+的沸腾6 mol/L硝酸溶液中浸泡96 h后的SEM像

图9 C25和304L不锈钢在含有不同浓度Mn2+的沸腾6 mol/L硝酸中浸泡96 h后表面各元素的XPS深度分布

图10 C25在含有不同浓度Mn2+的沸腾6 mol/L硝酸中浸泡96 h后表面溅射不同时间的Cr 2p、Fe 2p、Ni 2p和Mn 2p的精细谱

图11 304L在含有不同浓度Mn2+的沸腾6 mol/L硝酸中浸泡96 h后表面溅射不同时间的Cr 2p、Fe 2p、Ni 2p和Mn 2p的精细谱

表3 实验影响因素及水平设计

表4 C25不锈钢BBD模型的优化水平和Rp值

表5 304L不锈钢BBD模型的优化水平和Rp值

表6 C25和304L两种不锈钢的回归系数

表7 C25不锈钢BBD模型回归方差分析

表8 304L不锈钢BBD模型回归方差分析

图12 C25和304L不锈钢模型对响应值的预测值和真实值的关系

图13 C25和304L不锈钢的Rp值的摄动图

图14 温度、Mn2+浓度和硝酸浓度两两交互作用对C25不锈钢Rp的影响图及其对应的响应值的等高线图

图15 温度、Mn2+浓度和硝酸浓度两两交互作用对304L不锈钢Rp的影响图及其对应的响应值的等高线图

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