崔红兵,田世艳,张茂彩,王誉,杨金梦,辛博.电化学蚀刻-掺杂316L不锈钢制备PEMFC双极板[J].表面技术,2021,50(5):110-118, 167.
CUI Hong-bing,TIAN Shi-yan,ZHANG Mao-cai,WANG Yu,YANG Jin-meng,XIN Bo.Preparation of PEMFC Bipolar Plates by Electrochemical Etching-doping 316L Stainless Steel[J].Surface Technology,2021,50(5):110-118, 167
电化学蚀刻-掺杂316L不锈钢制备PEMFC双极板
Preparation of PEMFC Bipolar Plates by Electrochemical Etching-doping 316L Stainless Steel
投稿时间:2020-09-16  修订日期:2021-01-15
DOI:10.16490/j.cnki.issn.1001-3660.2021.05.011
中文关键词:  金属双极板  316L不锈钢  电化学处理  耐腐蚀  PEMFC
英文关键词:metal bipolar plate  316L stainless steel  electrochemical treatment  corrosion resistance  PEMFC
基金项目:北京市重点研究项目(Z17110000917010);白云稀土资源研究与综合利用国家重点试验室独立项目(2020Z2135)
作者单位
崔红兵 包头稀土研究院,内蒙古 包头 014030;瑞科稀土冶金及功能材料国家工程研究中心有限公司,内蒙古 包头 014030 
田世艳 中核北方核燃料元件有限公司,内蒙古 包头 014035 
张茂彩 包头稀土研究院,内蒙古 包头 014030;瑞科稀土冶金及功能材料国家工程研究中心有限公司,内蒙古 包头 014030 
王誉 包头稀土研究院,内蒙古 包头 014030;瑞科稀土冶金及功能材料国家工程研究中心有限公司,内蒙古 包头 014030 
杨金梦 北京科技大学,北京 100083 
辛博 包头稀土研究院,内蒙古 包头 014030;瑞科稀土冶金及功能材料国家工程研究中心有限公司,内蒙古 包头 014030 
AuthorInstitution
CUI Hong-bing Baotou Research Institute of Rare Earth, Baotou 014030, China;State Engineering Research Center of Rare Earth Metallurgy and Functional Materials, Baotou 014030, China 
TIAN Shi-yan China North Nuclear Fuel Co., Ltd, Baotou 014035, China 
ZHANG Mao-cai Baotou Research Institute of Rare Earth, Baotou 014030, China;State Engineering Research Center of Rare Earth Metallurgy and Functional Materials, Baotou 014030, China 
WANG Yu Baotou Research Institute of Rare Earth, Baotou 014030, China;State Engineering Research Center of Rare Earth Metallurgy and Functional Materials, Baotou 014030, China 
YANG Jin-meng University of Science and Technology Beijing, Beijing 100083, China 
XIN Bo Baotou Research Institute of Rare Earth, Baotou 014030, China;State Engineering Research Center of Rare Earth Metallurgy and Functional Materials, Baotou 014030, China 
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中文摘要:
      目的 研究在0.5 mol/L KNO3和0.1 mol/L HNO3混合溶液中,电极电位对316L不锈钢(316LSS)表层微观形貌、化学组成、耐腐蚀性能和界面接触电阻的影响,以解决316LSS双极板在质子交换膜燃料电池中服役时腐蚀和表面接触电阻较大的问题。方法 借助于电化学交流阻抗、循环伏安、计时电流和动电位极化测试,对316LSS表面发生的电化学反应及改性后性能进行研究。利用电化学工作站、扫描电镜及X射线光电子能谱分析仪,对316LSS的耐腐蚀性能、微观形貌及化合价进行表征,并测量界面接触电阻和反应后溶液中铁铬金属离子浓度进行测量。结果 在0.5 mol/L KNO3+0.1 mol/L HNO3的混合溶液中,316LSS表面发生的反应为不可逆过程,当改性电位为–0.5 V(vs. SCE)时,交流阻抗低频区出现了代表物质吸附的感抗弧,电位负移到–0.6 V(vs. SCE)和–0.7 V(vs. SCE)时,表面发生点腐蚀和晶界腐蚀,膜层的完整性被破坏。最佳电位–0.5 V(vs. SCE)改性后316LSS表面出现凸起结构,表层元素分析发现关键合金元素铬主要以氧化铬和氮化铬形式存在,–0.5 V(vs. SCE)对应的氮化铬占比达54.8%。在140 N/cm2的压力下界面接触电阻与施加电位呈现抛物线关系,最小电阻值为8.7 mΩ.cm2(–0.5 V(vs. SCE))。改性后的316LSS耐腐蚀性能显著提升,最佳样品的腐蚀电流密度和腐蚀电位分别为0.065 μA/cm2和136.738 mV,在模拟燃料电池中运行650 h时,腐蚀电流密度为3.4 μA/cm2。结论 电化学改性316LSS的物理化学性能与施加电位大小密切相关。由于316LSS表层钝化膜在电化学反应过程中发生选择性溶解以及原位氮掺杂,促使钝化膜厚度减薄,掺杂氮元素稳定了膜层结构和提高了导电性能,消除了钝化膜对双极板性能的不利影响。最佳改性电位下316LSS表面发生选择性蚀刻形成致密的凸起状氮掺杂膜层,改善了316L不锈钢双极板综合性能。
英文摘要:
      The effects of potential on the surface morphology, chemical composition, corrosion resistance, and interfacial contact resistance of 316L stainless steel (316LSS) in a mixed solution of 0.5 mol/L KNO3 and 0.1 mol/L HNO3 were studied to solve the problems of corrosion and high surface contact resistance of 316LSS bipolar plate in PEMFC. The electrochemical reaction and properties of 316LSS were studied by electrochemical impedance (EIS), cyclic voltammetry (CV), chronoamperometry, and potentiodynamic polarization tests. Electrochemical workstation, scanning electron microscope and X-ray photoelectron spectroscopy were used to characterize the corrosion resistance, microscopic morphology, and elemental valence of 316LSS, and the interface contact resistance and the concentration of Fe, Cr metal ions in the solution were measured. The reaction on the 316LSS surface is irreversible in the mixed 0.5 mol/L KNO3 + 0.1 mol/L HNO3 solution. EIS showed that there is an inductive impedance arc in the low frequency, and the 316LSS surface appeared to a convex structure under –0.5 V (vs. SCE). When the potential shifted to –0.6 V (vs. SCE) and –0.7 V (vs. SCE), pitting corrosion, and grain boundary corrosion occurred, and the integrity of the 316LSS surface is destroyed. The element analysis shows that the key alloy element chromium mainly exists in the chromium oxide and chromium nitride, the chromium nitride accounted for 54.8% (–0.5 V (vs. SCE)). The minimum resistance is 8.7 mΩ.cm2 at 140 N/cm2 (–0.5 V (vs. SCE)). The corrosion resistance of modified 316LSS is significantly improved, and the corrosion current density and corrosion potential of the best sample are 0.065 μA/cm2 and 136.738 mV, respectively. The corrosion current density was 3.4 μA/cm2 after 650 h operation in the durability test. The physical and chemical properties of modified 316LSS are closely related to the applied potential. Due to the selective dissolution of the 316LSS passivation film during the electrochemical reaction, and the thickness is reduced. The nitrogen doping stabilizes the passive film and improves the conductivity, thus eliminating the adverse effect of the passive film on the performance of the 316LSS bipolar plate. Under the optimal modified potential, the surface of 316LSS was selectively etched to form a dense nitrogen-doped film, which improved the comprehensive properties of 316L stainless steel bipolar plate.
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