质子交换膜燃料电池不锈钢双极板镀铌改性研究
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摘要
双极板是质子交换膜燃料电池的核心部件之一。本论文研究了采用对水和空气稳定的离子液体中对不锈钢进行电沉积铌,等离子体基离子注入铌的方法对不锈钢极性双极板进行改性,研究了膜层组织形貌和在模拟质子交换膜燃料电池(PEMFC)环境中的电化学性能和孔蚀动力学历程。
首先,采用离子液体1-乙基-3-甲基咪唑三氟甲磺酸盐作为电解质在304不锈钢上电沉积铌,铌镀层以孤岛的形式均匀分布在不锈钢表面,其高度在100nm以内。镀铌后304不锈钢表面生成化学惰性良好的NbO、Nb2O5,所形成的一层氧化铌惰性薄保护膜覆盖着基体。在模拟PEMFC的环境中,镀铌304不锈钢的腐蚀电位提高,电化学极化性能得到改善,反应电阻增大,提高了耐蚀性能。
其次,首次采用氯化胆碱类离子液体氯化胆碱-乙二醇为电解质在316不锈钢上电沉积铌,获得平整均匀的颗粒状镀层。铌镀层以孤岛的形式均匀分布在不锈钢表面,其高度在50nm以内。镀铌后316表面生成化学惰性良好的NbO、Nb2O5,改善了316不锈钢表面膜的钝化能力。在模拟PEMFC环境中,镀铌后316不锈钢的维钝电流密度减小,改善了阳极极化性能；孔蚀电位正移,反应电阻增大,提高了耐蚀性能。以对水和空气稳定的氯化胆碱类离子液体为电解质进行电镀,镀液性质稳定,可重复利用,绿色环保。
最后,采用金属等离子体基离子注入技术对316不锈钢进行铌离子注入,发现注入铌层以孤岛的形式均匀分布在不锈钢表面,其高度在50nm以内。离子注入铌后316不锈钢表面形成的化学惰性良好的NbO2、Nb2O5膜层及弥散的铌的氧化物小颗粒析出相的化学效应,使其基体的电化学性能得到提高。在模拟PEMFC环境中电化学测试结果,离子注入铌316不锈钢的腐蚀电位升高,维钝电流密度减小,电荷转移电阻增大,电容值降低,注入铌层成为高电阻、低电容的阻挡层,增强了不锈钢表面钝化能力,抑制和减缓了腐蚀反应。在85℃的模拟PEMFC阳极和阴极环境中,离子注入铌316不锈钢腐蚀动力学方程分别为i0-556.85.t-1/2和i0=1108.17.t-1/2,表明孔蚀过程受孔表面盐膜溶解控制。
The bipolar plate is one of the critical components of a proton-exchange-membrane fuel cell (PEMFC). In this study, niobium electrodeposited on stainless steel from air-and water-stable ionic liquids and niobium implanting on stainless steel bipolar plate by metal plasma immersion ion implantation (MePBII) have been researched. The niobium film morphology, electrochemical properties and pitting dynamics course are investigated in the simulated PEMFC environment.
Firstly, an air-and water-stable ionic liquid,1-ethyl-3-methylimidazolium trifluoromethane sulfonate ([Emim]OTF), has been applied as electrolytes for niobium electrodeposition for the first time. The electrochemical behavior of bare and niobium coated304stainless steel are evaluated by electrochemical tests in PEMFC environment. The results show that niobium can be electrodeposited on the surface of stainless steel in the ionic liquid electrolyte. The niobium plating roughness is within100nm and a thin niobium film acted as barrier can remarkably improve the corrosion resistance of304stainless steel in the PEMFC environment. The analysis of X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Atomic force microscopy (AFM) indicate that the improvement is attributed to the smoothness and strong chemical stability of NbO, Nb2O5film.
Subsequently, another water and air-stable choline chloride based ionic liquid, choline chloride-ethylene glycol, has been explored as an electrolyte for niobium electrodeposition on316stainless steel for the first time. A uniform-dense(isolated island-like) niobium film is obtained on316stainless steel surface. The plating roughness is within50nm. The coated niobium form chemically inert compounds of NbO and Nb2O5which behave as an anti-corrosion barrier and improve the passavition ability of surface layer. The results of the electrochemical characteristic indicate that in simulated PEMFC environment, the electrochemical characteristics of316stainless steel are improved greatly after coated with niobium such as corrosion potential increasing, passivation current density decreasing, pitting potential moving toward positive, and reaction resistance enlarging. ionic liquids electrolytes has obvious advantages such as higher character stability, non-pollution, reusable, less side reactions, and wide usage prospects.
Finally, niobium implanting on316stainless steel by metal plasma immersion ion implantation (MePBII) has been investigated. The plating roughness of niobium deposited films is within50nm. The electrochemical results reveal that, compared with uncoated substrates, corrosion potential and reaction resistance increases, passivation current density decreases, and pitting potential moves toward positive. The corrosion resistance of the Nb implanted316stainless steel has been improved significantly. The Nb coating was an effective barrier with high resistance and low capacitance which against the inward penetration of corrosive species. This can be attributed to niobium as effectively resistant to pitting corrosion and has more stable chemical properties. the ion implantation niobium316stainless steel corrosion kinetics equations isi0=-556.85.t12and i0=1108.17.t12respectively. It shows that pitting process is controlled by film dissolution.
首先,采用离子液体1-乙基-3-甲基咪唑三氟甲磺酸盐作为电解质在304不锈钢上电沉积铌,铌镀层以孤岛的形式均匀分布在不锈钢表面,其高度在100nm以内。镀铌后304不锈钢表面生成化学惰性良好的NbO、Nb2O5,所形成的一层氧化铌惰性薄保护膜覆盖着基体。在模拟PEMFC的环境中,镀铌304不锈钢的腐蚀电位提高,电化学极化性能得到改善,反应电阻增大,提高了耐蚀性能。
其次,首次采用氯化胆碱类离子液体氯化胆碱-乙二醇为电解质在316不锈钢上电沉积铌,获得平整均匀的颗粒状镀层。铌镀层以孤岛的形式均匀分布在不锈钢表面,其高度在50nm以内。镀铌后316表面生成化学惰性良好的NbO、Nb2O5,改善了316不锈钢表面膜的钝化能力。在模拟PEMFC环境中,镀铌后316不锈钢的维钝电流密度减小,改善了阳极极化性能；孔蚀电位正移,反应电阻增大,提高了耐蚀性能。以对水和空气稳定的氯化胆碱类离子液体为电解质进行电镀,镀液性质稳定,可重复利用,绿色环保。
最后,采用金属等离子体基离子注入技术对316不锈钢进行铌离子注入,发现注入铌层以孤岛的形式均匀分布在不锈钢表面,其高度在50nm以内。离子注入铌后316不锈钢表面形成的化学惰性良好的NbO2、Nb2O5膜层及弥散的铌的氧化物小颗粒析出相的化学效应,使其基体的电化学性能得到提高。在模拟PEMFC环境中电化学测试结果,离子注入铌316不锈钢的腐蚀电位升高,维钝电流密度减小,电荷转移电阻增大,电容值降低,注入铌层成为高电阻、低电容的阻挡层,增强了不锈钢表面钝化能力,抑制和减缓了腐蚀反应。在85℃的模拟PEMFC阳极和阴极环境中,离子注入铌316不锈钢腐蚀动力学方程分别为i0-556.85.t-1/2和i0=1108.17.t-1/2,表明孔蚀过程受孔表面盐膜溶解控制。
The bipolar plate is one of the critical components of a proton-exchange-membrane fuel cell (PEMFC). In this study, niobium electrodeposited on stainless steel from air-and water-stable ionic liquids and niobium implanting on stainless steel bipolar plate by metal plasma immersion ion implantation (MePBII) have been researched. The niobium film morphology, electrochemical properties and pitting dynamics course are investigated in the simulated PEMFC environment.
Firstly, an air-and water-stable ionic liquid,1-ethyl-3-methylimidazolium trifluoromethane sulfonate ([Emim]OTF), has been applied as electrolytes for niobium electrodeposition for the first time. The electrochemical behavior of bare and niobium coated304stainless steel are evaluated by electrochemical tests in PEMFC environment. The results show that niobium can be electrodeposited on the surface of stainless steel in the ionic liquid electrolyte. The niobium plating roughness is within100nm and a thin niobium film acted as barrier can remarkably improve the corrosion resistance of304stainless steel in the PEMFC environment. The analysis of X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Atomic force microscopy (AFM) indicate that the improvement is attributed to the smoothness and strong chemical stability of NbO, Nb2O5film.
Subsequently, another water and air-stable choline chloride based ionic liquid, choline chloride-ethylene glycol, has been explored as an electrolyte for niobium electrodeposition on316stainless steel for the first time. A uniform-dense(isolated island-like) niobium film is obtained on316stainless steel surface. The plating roughness is within50nm. The coated niobium form chemically inert compounds of NbO and Nb2O5which behave as an anti-corrosion barrier and improve the passavition ability of surface layer. The results of the electrochemical characteristic indicate that in simulated PEMFC environment, the electrochemical characteristics of316stainless steel are improved greatly after coated with niobium such as corrosion potential increasing, passivation current density decreasing, pitting potential moving toward positive, and reaction resistance enlarging. ionic liquids electrolytes has obvious advantages such as higher character stability, non-pollution, reusable, less side reactions, and wide usage prospects.
Finally, niobium implanting on316stainless steel by metal plasma immersion ion implantation (MePBII) has been investigated. The plating roughness of niobium deposited films is within50nm. The electrochemical results reveal that, compared with uncoated substrates, corrosion potential and reaction resistance increases, passivation current density decreases, and pitting potential moves toward positive. The corrosion resistance of the Nb implanted316stainless steel has been improved significantly. The Nb coating was an effective barrier with high resistance and low capacitance which against the inward penetration of corrosive species. This can be attributed to niobium as effectively resistant to pitting corrosion and has more stable chemical properties. the ion implantation niobium316stainless steel corrosion kinetics equations isi0=-556.85.t12and i0=1108.17.t12respectively. It shows that pitting process is controlled by film dissolution.
引文
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