摘要
本博士学位论文利用电化学沉积法制备了两种含配位稀土离子甘氨酸合铕(Eu(Ⅲ)(Gly)x)和邻苯二甲酸合钕(Nd(Ⅲ)(o-phth)x)成份的金属杂多核氰桥混配聚合物化学修饰铂电极,在此基础上研究了此类修饰电极的电催化行为、并探讨了其在分析应用方面的特性。论文的主要内容如下：
1、利用电化学沉积法成功制备了铕-铁-铬酸根类普鲁士蓝修饰铂电极。用扫描电子显微镜(SEM)、傅立叶变换红外光谱(FT-IR)、傅立叶变换拉曼光谱(FT-Raman)、固体表面荧光等技术对修饰物的材料性质进行了表征。用循环伏安法(CV)、方波伏安法(SWV)研究了该聚合物修饰铂电极上Ru(bpy)32+的电催化氧化行为。发现在0.40mol/L的硝酸钾电解质溶液中,Ru(bpy)32+在这种无机聚合物修饰铂电极上呈现出稳定、良好的电催化氧化伏安特性,用方波伏安法测得其催化氧化峰电流与Ru(bpy)32+浓度在0.001-1.0mmol/L范围内呈现良好的线性关系,其催化氧化效率提高至裸铂电极的3.5倍左右。同时发现,该修饰电极上发光探针分子Ru(bpy)32+的ECL总发光强度也相应得到提高。据此,提出了一个可以合理解释修饰电极表面上Ru(bpy)32+电致化学发光现象的新机理模型。作为分析应用可能性探索,发现当此修饰电极作为柱端电致化学发光-毛细管电泳联用分析仪的检测工作电极时,可使CE-ECL法检测探针物质三丙胺(TrPA)和三乙胺(TEA)样品的分析灵敏度提高约1个数量级。
2、用电沉积法成功制备了一种新型的钕-铁-钼酸根金属杂多核氰桥配位聚合物修饰铂电极(Nd(Ⅲ)(o-phth)x-Fe-MoO42-/Pt),用扫描电子显微镜(SEM)、傅立叶变换红外光谱(FT-IR)、傅立叶变换拉曼光谱(FT-Raman)、X-ray粉末衍射(XRD)等技术对修饰物的材料性质进行了表征,并研究了此修饰电极的电催化活性和对CO等毒性中间体的耐受能力。采用弱酸性介质,用循环伏安法(CV)和计时安培法(CA)研究发现,乙醇在此钕-铁-钼酸根类普鲁士蓝修饰电极上的电催化氧化反应有5个明显的伏安峰存在。伏安法实验数据分析表明,阴极化扫描过程中乙醇的反扫氧化峰具有扩散控制的动力学特征,其成因可能源于乙醇经一步协同脱氢形成乙醛的反应。在此基础上推断乙醇在该修饰电极上可能遵循不同的脱氢机理,提出了一个可合理解释乙醇电催化氧化反应的脱氢机理新模型。
3、以两步电化学沉积法成功制备了新型铂微粒/钕-铁-钼酸根类普鲁士蓝复合修饰铂电极(Pt-particle/Nd(Ⅲ)(o-phth)x-Fe-MoO42-/Pt),用循环伏安法(CV)和计时安培法(CA)研究了甲醇在该类普鲁士蓝复合修饰铂电极上的伏安行为。实验结果表明,在钕-铁-钼酸根类普鲁士蓝修饰电极基底上,由于铂微粒的分散均匀度好、铂的担载量适中,该复合修饰铂电极对甲醇有高效的电催化氧化作用。在弱酸性条件下,对0.25mol/L甲醇而言,其阳极化扫描过程中甲醇催化氧化峰的最高电流密度可达到120mA/cm2。此外,根据伏安实验数据分析,对涉及甲醇氧化反应四个相关伏安峰的性质分别给出了合理的解释。以此为据,推断甲醇在铂微粒/钕-铁-钼酸根类普鲁士蓝复合修饰铂电极的脱氢过程符合PtOH中间体促进下的多步单电子转移机理模型。
In the doctoral thesis, two kinds of platinum electrodes which were chemically modified with the hybrid-metallic cyano-bridged mixed coordination polymers containing the composition of the europium-glycine complex (Eu(Ⅲ)Gly)x) and the neodymium-phthalic acid complex (Nd(Ⅲ)(o-phth)x) were prepared respectively by electrodeposition methods. Furthermore, the electrocatalytic behavior of such a modified electrode was investigated and their characteristics in applications of analytical chemistry were explored. The main content of the paper is as follows:
1. A platinum electrode modified with the Eu(Ⅲ)Gly)x-Fe-CrO42-coordination polymer was prepared successfully by electrodeposition methods. The scanning electron microscope (SEM), FT-IR, FT-Raman, and solid surface reflect fluorescence techniques were used to characterize properties of the modified material. The electrocatalytic oxidation behavior of tris(2,2'-bipyridyl)-ruthenium(II)(Ru(bpy)32+) was investigated in detail on the modified platinum electrode (Eu(Ⅲ)(Gly)x-Fe-CrO42-/Pt) by cyclic voltammetry (CV) and square wave voltammetry (SWV). In the electrolyte containing0.45mol/L potassium nitrate, Ru(bpy)32+exhibited the stable and good electrocatalytic oxidation characteristic on the Eu(Ⅲ)(Gly)x-Fe-CrO42-/Pt, and a linear relationship between the square wave peak current and Ru(bpy)32+concentration was shown in the range of0.001～1.0mmol/L. The catalytic oxidation efficiency of Ru(bpy)32+increased to3.5times on the modified platinum electrode comparing with its values on the bare platinum electrode. In addition, it was discovered that because of the enhancement of catalytic oxidation efficiency on the modified electrode surface, the total electrochemiluminescence intensity of Ru(bpy)32+system also increased under the same experimental condition. Based on the above evidences, a novel mechanism model was proposed to interpret the ECL behavior of Ru(bpy)32+system on the modified platinum electrode. As a possible analytical application for capillary electrophoresis coupled with end-column electrochemiluminescence detection, it was testified that when modified platinum electrode was used as a detector's working electrode, the sensitivity of CE-ECL for determining the probe samples containing tripropylamine (TrPA) and triethylamine (TEA) was positively improved by about one order of magnitude.
2. A novel modified platinum electrode (Nd(Ⅲ)(o-phth)x-Fe-MoO42-/Pt) was prepared by electrodeposition methods. The scanning electron microscope (SEM), FT-IR, FT-Raman, and X-ray powder diffraction (XRD) techniques were used to characterize properties of the modified material. The electrocatalytic activity and CO-poisoning tolerance of the modified electrode had been studied on the decorated polycrystalline platinum surface for ethanol electrooxidation. In addition, the electrocatalytic oxidation of ethanol was studied in detail by using cyclic voltammetry (CV) and chronoamperometry (CA) in a weakly acidic condition, and the presence of five distinct current peaks related to the ethanol electrooxidation process was observed. From the voltammetric data analysis, the kinetic behavior of backward oxidation peak in negative-going sweep was considered to be a diffusion-controlled electrochemical process. Therefore, the nature of backward oxidation peak was reasonably attributed to the plentiful products of acetaldehyde via a one-step concerted dehydrogenation pathway of ethanol. These results implied that the electrooxidation of ethanol possibly had different dehydrogenation pathways on the decorated platinum electrode comparing with normal ones. Based on the particular experimental evidences, a new dehydrogenation model was proposed to explain preliminarily the mechanism of ethanol electrooxidation.
3. A composite modified platinum electrode (Pt-particles/Nd(Ⅲ)(o-phth)x-Fe-MoO42-/Pt) was successfully prepared by the two-step electrodeposition method. The voltammetric behavior of methanol on the Pt-particle/Nd(Ⅲ)(o-phth)x-Fe-MoO42-/Pt composite modified electrode was studied by cyclic voltammetry (CV) and chronoamperometry (CA). The experimental results showed that because of the good dispersive uniformity and the feasible carrying capacity of Pt-particles on the modified electrode substrate, the high efficient electrocatalytic activity for methanol oxidation was available at the composite modified electrode. Under a weakly acidic condition, the current density of main oxidation peak in positive-going sweep for0.25mol/L methanol could achieve up to120mA/cm2. Furthermore, from the analysis to voltammetric data, the nature of four voltammetric peaks relating to the oxidation reaction of methanol was revealed respectively with a reasonable explanation. Therefore, it was inferred that the dehydrogenation mechanism of methanol on Pt-particles/Nd(Ⅲ)(o-phth)x-Fe-MoO42-/Pt electrode would undergo a multi-step single electron transfer process which was promoted by PtOH active intermediates.
引文
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