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Solid molybdenum nitride microdisc electrodes: Fabrication, characterisation, and application to the reduction of peroxodisulfate
Electrochimica Acta ( IF 6.6 ) Pub Date : 2018-10-08 , DOI: 10.1016/j.electacta.2018.10.046
Saiful Arifin Bin Shafiee , Andrew L. Hector , Guy Denuault

A new methodology was developed to fabricate solid molybdenum nitride microdisc electrodes for the first time. The MoN microrods were produced by heating Mo microwires in dry NH3 atmosphere for several hours. They were characterised by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD). The latter revealed the samples had crystallised in the δ3-MoN phase with a core of γ-Mo2N. Their electrochemical behaviour was probed for the reduction of Ru(NH3)63+. For this fast electron transfer the MoN microdisc electrodes returned similar voltammetric features to Pt microelectrodes. Their amperometric response was further tested with the reduction of peroxodisulfate. In contrast with other electrode materials, the reduction of S2O82− on MoN microdiscs delivered steady state voltammograms with well-defined diffusion controlled plateau. At low sweep rates, the limiting current was consistent with hemispherical diffusion and stable for at least 500 s. The diffusion coefficient of S2O82− derived from these results, 9.5 × 10−6 cm2 s−1, is in excellent agreement with previous work. At high sweep rates, the reduction of peroxodisulfate was found to be complicated by the simultaneous reduction of adsorbates. The results indicate that MoN is an ideal electrode material to monitor the concentration of peroxodisulfate under steady state conditions.



中文翻译:

固态氮化钼微盘电极:制备,表征及其在还原过二硫酸盐中的应用

开发了一种新的方法来首次制造固态氮化钼微盘电极。通过在干燥的NH 3气氛中加热Mo微丝数小时来生产MoN微棒。它们的特征在于扫描电子显微镜(SEM),能量色散光谱(EDS)和X射线衍射(XRD)。后者揭示了在样品中δ结晶3 -Mon相用γ-沫的芯2 N.它们的电化学行为进行了探查的Ru(NH的还原36 3+。为了实现这种快速的电子传输,MoN微盘电极向Pt微电极返回了相似的伏安特征。用过二硫酸盐的减少进一步测试了它们的安培响应。与其他电极材料相比,MoN微盘上S 2 O 8 2-的还原提供了具有明确定义的扩散控制平台的稳态伏安图。在低扫描速率下,极限电流与半球形扩散一致,并且稳定至少500 s。由这些结果得出的S 2 O 8 2-的扩散系数为9.5×10 -6  cm 2  s -1,与以前的工作非常吻合。在高吹扫速率下,发现过氧二硫酸盐的还原由于同时减少吸附物而变得复杂。结果表明,MoN是监测稳态条件下过二硫酸盐浓度的理想电极材料。

更新日期:2018-10-08
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