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In Situ Characterization of Ni and Ni/Fe Thin Film Electrodes for Oxygen Evolution in Alkaline Media by a Raman-Coupled Scanning Electrochemical Microscope Setup
Analytical Chemistry ( IF 6.7 ) Pub Date : 2017-10-04 00:00:00 , DOI: 10.1021/acs.analchem.7b01060 Matthias Steimecke 1 , Gerda Seiffarth 1 , Michael Bron 1
Analytical Chemistry ( IF 6.7 ) Pub Date : 2017-10-04 00:00:00 , DOI: 10.1021/acs.analchem.7b01060 Matthias Steimecke 1 , Gerda Seiffarth 1 , Michael Bron 1
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We present a spectroelectrochemical setup, in which Raman microscopy is combined with scanning electrochemical microscopy (SECM) in order to provide both spectroscopic and electrochemical information on the very same location of an electrode at the same time. The setup is applied to a subject of high academic and practical interest, namely, the oxygen evolution reaction at Ni and Ni/Fe electrodes. It comprises a transparent substrate electrode, onto which Ni and Ni/Fe thin films are deposited. An ultramicroelectrode (UME) is placed closely above the substrate to obtain electrochemical information, while a Raman microscope probes the same sample spot from below. To obtain information on oxygen evolution activity and structural changes, increasingly positive potentials from 0.1 up to 0.7 V vs Hg|HgO|1 M KOH were applied to the Ni/Fe-electrodes in 0.1 M KOH solution. Evolved oxygen is detected by reduction at a Pt UME, allowing for the determination of onset potentials, while the substrate current, which is recorded in parallel, is due to both overlapping oxygen evolution and the oxidation of Ni(OH)2 to NiOOH. An optimum of 15% Fe in Ni/Fe films with respect to oxygen evolution activity was determined. At the same time, the potential-dependent formation of γ-NiOOH characterized by the Raman double band at 475 and 557 cm–1 allows for the conclusion that a certain amount of disorder introduced by Fe atoms is necessary to obtain high oxygen evolution reaction (OER) activity.
中文翻译：
Ni和Ni / Fe薄膜电极的原位表征，用于通过碱性拉曼耦合扫描电化学显微镜对氧气在碱性介质中的析出
我们提出了一种光谱电化学装置，其中拉曼显微镜与扫描电化学显微镜（SECM）相结合，以便同时在电极的同一位置提供光谱和电化学信息。该装置适用于具有高度学术和实践意义的主题，即Ni和Ni / Fe电极上的氧气逸出反应。它包括一个透明的衬底电极，其上沉积有Ni和Ni / Fe薄膜。将超微电极（UME）紧紧置于基板上方以获得电化学信息，而拉曼显微镜则从下方探测相同的样品点。为了获得有关氧释放活性和结构变化的信息，将相对于Hg | HgO | 1 M KOH从0.1到0.7 V的正电势逐渐应用于0的Ni / Fe电极。1 M KOH溶液。通过在Pt UME上还原可检测出析出的氧气，从而可确定发病电位，同时衬底电流，其被记录在平行的，是因为这两个重叠的析氧和Ni（OH）的氧化2到的NiOOH。确定了相对于氧气析出活性，Ni / Fe薄膜中15％Fe的最佳值。同时，以475和557 cm –1处的拉曼双能带为特征的γ-NiOOH的电势依赖性形成可以得出这样的结论，即为了获得高氧释放反应，Fe原子引入一定量的无序性是必要的（ OER）活动。
更新日期：2017-10-04
中文翻译：
Ni和Ni / Fe薄膜电极的原位表征，用于通过碱性拉曼耦合扫描电化学显微镜对氧气在碱性介质中的析出
我们提出了一种光谱电化学装置，其中拉曼显微镜与扫描电化学显微镜（SECM）相结合，以便同时在电极的同一位置提供光谱和电化学信息。该装置适用于具有高度学术和实践意义的主题，即Ni和Ni / Fe电极上的氧气逸出反应。它包括一个透明的衬底电极，其上沉积有Ni和Ni / Fe薄膜。将超微电极（UME）紧紧置于基板上方以获得电化学信息，而拉曼显微镜则从下方探测相同的样品点。为了获得有关氧释放活性和结构变化的信息，将相对于Hg | HgO | 1 M KOH从0.1到0.7 V的正电势逐渐应用于0的Ni / Fe电极。1 M KOH溶液。通过在Pt UME上还原可检测出析出的氧气，从而可确定发病电位，同时衬底电流，其被记录在平行的，是因为这两个重叠的析氧和Ni（OH）的氧化2到的NiOOH。确定了相对于氧气析出活性，Ni / Fe薄膜中15％Fe的最佳值。同时，以475和557 cm –1处的拉曼双能带为特征的γ-NiOOH的电势依赖性形成可以得出这样的结论，即为了获得高氧释放反应，Fe原子引入一定量的无序性是必要的（ OER）活动。
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