A microwave‐assisted solvothermal method is proposed as a rapid and low‐cost fabrication procedure of RuO₂ nanoparticles using citric acid as stabilizing agent in ethylene glycol, and H₂O₂ as oxidizing agent at 180 °C. Structural and morphological characterizations of the powder are investigated using X‐Ray diffraction (XRD), scanning electronic microscopy (SEM) and transmission electron microscopy (TEM). XRD analysis shows that there is a synergic effect to obtain RuO₂ nanoparticles when 6% v/v H₂O₂ is added followed by a calcination of the powder, due to reactive oxygen intermediates (¹O₂, HO⁻₂, HO^•₂, ^•OH) generated in the first stage. TEM and SEM images of as‐synthesized material exhibit an uniform particle distribution (PSD) of RuO₂ nanoparticles with averaged diameter of ca. 38 nm, and its indexing indicates the RuO₂ stoichiometry with high degree of crystallinity. The preliminary electrocatalytic performance of RuO₂ nanoparticles coated on Ti is investigated using voltammetry and electrochemical impedance spectroscopy (EIS), towards the oxygen (OER) and chlorine evolution reaction (CER) in 1 mol L⁻¹ H₂SO₄ and 0.1 mol L⁻¹ NaCl, respectively. Cyclic voltammograms of RuO₂ display typical behaviors for OER and CER at 1.25 and 1.1 V vs Ag/AgCl, respectively. A Tafel slope of 44 mV dec⁻¹ corrected for ohmic drop was obtained in sulfate media which confirmed the OER mechanism in the absence of chlorides; while this parameter is around 25 mV dec⁻¹ in NaCl (CER), strongly depending on the chloride concentration and the extent of OER input. In NaCl media, the energy barriers represented by the charge transfer resistances for CER are overcome at more positive potentials than for OER, and a greater activity of the O₂ evolution is observed as the potential became more positive.

中文翻译：

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微波辅助溶剂热一锅法合成RuO2纳米颗粒：其对氧和氯发生反应的活性的初步见解

提出了一种微波辅助溶剂热法，以柠檬酸为乙二醇稳定剂，H ₂ O ₂为氧化剂，在180°C下快速低成本制备RuO ₂纳米颗粒。使用X射线衍射（XRD），扫描电子显微镜（SEM）和透射电子显微镜（TEM）研究了粉末的结构和形态特征。XRD分析表明，有协同作用，得到的RuO ₂纳米颗粒时6％V / Vħ ₂ ö ₂，然后加入粉末的煅烧，由于活性氧中间体（¹ Ò ₂，HO ^- ₂，HO ^• ₂，^• OH）在第一阶段生成。合成后的材料的TEM和SEM图像显示出RuO ₂纳米颗粒的均匀颗粒分布（PSD），平均直径约为。38 nm，其分度表明具有高度结晶度的RuO ₂化学计量。使用伏安法和电化学阻抗谱（EIS）研究了涂在Ti上的RuO ₂纳米颗粒对1 mol L ^-1 H ₂ SO ₄和0.1 mol L中的氧气（OER）和氯生成反应（CER）的初步电催化性能。^-1 NaCl分别。RuO的循环伏安图_图2显示了OER和CER分别在1.25和1.1 V相对于Ag / AgCl的典型行为。在硫酸盐介质中获得针对欧姆滴校正的44 mV dec ^-1的Tafel斜率，证实了在不存在氯化物的情况下的OER机制；而该参数在NaCl（CER）中约为25 mV dec ^-1，这在很大程度上取决于氯化物浓度和OER输入的程度。在NaCl介质中，以比OER更高的正电势克服了CER的电荷转移电阻所代表的能垒，并且随着电势变得更正，可以观察到O ₂析出的活性更高。