电催化材料制备、表征及应用
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摘要
电催化反应是电化学研究重要课题,当电极反应中存在催化剂时,反应活化能降低、反应速率提高。改善电极材料是实现电催化过程的重要手段。本文以寻找高活性电催化材料为目标,比较系统地就电催化析氢材料、甲醇电催化氧化及修饰碳糊电极进行了研究。
基于复合电沉积技术将La_2O_3掺杂到钛基镍钴合金镀层中,采用扫描电子显微镜及X-射线衍射表征复合材料的形貌和微观结构。采用稳态极化曲线、Tafel曲线及电化学阻抗谱评价复合材料析氢性能。结果表明,掺杂La_2O_3能提高复合镀层电极表面粗糙度及表面积,当电流密度为15.0mA·cm–2时,相对于镍-钴合金涂层电极,镍-钴-La_2O_3复合电极析氢电位正移178mV。镍-钴-La_2O_3复合电极是一种具有较高电催化析氢活性的材料。
考察制备条件对甲醇电氧化催化剂粒径的影响,进而考察对电催化活性影响。采用浸渍还原法制备纳米结构Pt/C电催化剂,采用X-射线衍射、循环伏安法、交流阻抗法、计时电流法考察常见有机溶剂(乙醇、丙酮、异丙醇、正丁醇)对酸性溶液体系中甲醇氧化催化性能的影响。基于添加辅助催化剂的思路,将多孔沸石掺杂到Pt/C催化剂中,采用电化学方法评价修饰催化剂对甲醇氧化电催化性能。结果表明,掺入多孔沸石可提高催化剂对甲醇电催化氧化活性。
以新型细菌纤维素纳米碳纤维用作碳糊电极碳材料,制得细菌纤维素碳糊电极,采用扫描电子显微镜、循环伏安法、交流阻抗法等方法表征所得碳糊电极的性能。结果表明,与传统电极相比,细菌纤维素碳糊电极在Fe(CN)_6~(3-/4-)氧化还原体系中的氧化还原峰峰电流更大,峰电位差更小,电荷传递电阻更小。基于此,采用循环伏安扫描在细菌纤维素电极表面自组装磷钼酸,制得磷钼酸修饰细菌纤维素碳糊电极,研究修饰电极的电化学行为,发现电极在硫酸与硫酸钠混合溶液中具有较好的稳定性,同时,对亚硝酸盐具有很好的电催化还原作用。
Electrocatalytic reactions are important aspects of electrochemical investigation. When the electrode reactions occurred in the presence of electrocatalyts, the activation ergegy would be decreased and the reaction rate would be enhanced. In order to find materials with high electrocatalytic activity, the hydrogen evolution electrocatalytic materials, electrocatalytic oxidation to methanol and modified carbon paste electrode were studied.
Firstly, La_2O_3 was successfully doped into nickel-cobalt alloy coating on Ti substrate by electrodeposition technology. The surface morphology and microstructure were examined by SEM and XRD, respectively, and the hydrogen evolution property was evaluated by steady-state polarization, Tafel plot and electrochemical impedance spectroscopy. It was found that the incorporated La_2O_3 particles resulted in the improvement of roughness and surface area of the composite coating electrode, and hydrogen evolution potential of nickel-cobalt-La_2O_3 composite coating electrode moved positively around 178 mV at 15.0 mA cm–2 compared with that of nickel-cobalt alloy deposited coating electrode. The proposed materials are promising hydrogen evolution electrocatalytic materials.
Nanostructured Pt/C catalyst for methanol electrooxidation was prepared by impregnation method in different water-organic solvents (ethanol, acetone, isopropanol, n-butanol). It was found that the size of Pt particle was varied with water-organic solvents demonstrated by XRD. Its electrocatalytic activity to methanol was evaluated by cyclic voltammetry, electrochemical impedance spectroscopy and chronoamperometry. Due to that the electroactivity of catalyst could be enhanced by adding assistant electrocatalysts, the 4A-zeolite as assistant electrocatalyst was doped into Pt/C catalyst by simple mixing. The corresponding electrocatalytic activity for electrooxidation of methanol was evaluated in alkaline medium by several electrochemical techniques, including cyclic voltammetry, electrochemical impedance spectroscopy and chronoamperometry. It was shown that the electrocatalytic activity of the 4A-zeolite modified Pt/C catalyst was much better than that of the Pt/C catalyst. The increased electrocatalytic activity could be attributed to that the advanced properties of the micrometer 4A-zeolite with nano-porosity could significantly increase the effective electrode surface and facilitate the diffusion of analytes into the film of electrode surface.
Carbonized bacterial cellulose based carbon paste electrode (BCPE) was fabricated with nano-dimension carbonized bacterial cellulose (BC) fiber and studied by SEM, cyclic voltammetry and electrochemical impedance spectroscopy. Compared with traditional carbon paste electrode (CPE), a faster electron-transfer kinetics process happened on BCPE in wide scan rate ranges. Moreover, PMo12 was successfully assembled on BCPE surface by cyclic voltametric scanning method. Good stability and catalytic activity to the reduction of nitrite were observed on PMo12/BCPE. This novel carbonaceous materials is prospected to be used in electrocatalysis and other fields due to its mentioned advantages.
基于复合电沉积技术将La_2O_3掺杂到钛基镍钴合金镀层中,采用扫描电子显微镜及X-射线衍射表征复合材料的形貌和微观结构。采用稳态极化曲线、Tafel曲线及电化学阻抗谱评价复合材料析氢性能。结果表明,掺杂La_2O_3能提高复合镀层电极表面粗糙度及表面积,当电流密度为15.0mA·cm–2时,相对于镍-钴合金涂层电极,镍-钴-La_2O_3复合电极析氢电位正移178mV。镍-钴-La_2O_3复合电极是一种具有较高电催化析氢活性的材料。
考察制备条件对甲醇电氧化催化剂粒径的影响,进而考察对电催化活性影响。采用浸渍还原法制备纳米结构Pt/C电催化剂,采用X-射线衍射、循环伏安法、交流阻抗法、计时电流法考察常见有机溶剂(乙醇、丙酮、异丙醇、正丁醇)对酸性溶液体系中甲醇氧化催化性能的影响。基于添加辅助催化剂的思路,将多孔沸石掺杂到Pt/C催化剂中,采用电化学方法评价修饰催化剂对甲醇氧化电催化性能。结果表明,掺入多孔沸石可提高催化剂对甲醇电催化氧化活性。
以新型细菌纤维素纳米碳纤维用作碳糊电极碳材料,制得细菌纤维素碳糊电极,采用扫描电子显微镜、循环伏安法、交流阻抗法等方法表征所得碳糊电极的性能。结果表明,与传统电极相比,细菌纤维素碳糊电极在Fe(CN)_6~(3-/4-)氧化还原体系中的氧化还原峰峰电流更大,峰电位差更小,电荷传递电阻更小。基于此,采用循环伏安扫描在细菌纤维素电极表面自组装磷钼酸,制得磷钼酸修饰细菌纤维素碳糊电极,研究修饰电极的电化学行为,发现电极在硫酸与硫酸钠混合溶液中具有较好的稳定性,同时,对亚硝酸盐具有很好的电催化还原作用。
Electrocatalytic reactions are important aspects of electrochemical investigation. When the electrode reactions occurred in the presence of electrocatalyts, the activation ergegy would be decreased and the reaction rate would be enhanced. In order to find materials with high electrocatalytic activity, the hydrogen evolution electrocatalytic materials, electrocatalytic oxidation to methanol and modified carbon paste electrode were studied.
Firstly, La_2O_3 was successfully doped into nickel-cobalt alloy coating on Ti substrate by electrodeposition technology. The surface morphology and microstructure were examined by SEM and XRD, respectively, and the hydrogen evolution property was evaluated by steady-state polarization, Tafel plot and electrochemical impedance spectroscopy. It was found that the incorporated La_2O_3 particles resulted in the improvement of roughness and surface area of the composite coating electrode, and hydrogen evolution potential of nickel-cobalt-La_2O_3 composite coating electrode moved positively around 178 mV at 15.0 mA cm–2 compared with that of nickel-cobalt alloy deposited coating electrode. The proposed materials are promising hydrogen evolution electrocatalytic materials.
Nanostructured Pt/C catalyst for methanol electrooxidation was prepared by impregnation method in different water-organic solvents (ethanol, acetone, isopropanol, n-butanol). It was found that the size of Pt particle was varied with water-organic solvents demonstrated by XRD. Its electrocatalytic activity to methanol was evaluated by cyclic voltammetry, electrochemical impedance spectroscopy and chronoamperometry. Due to that the electroactivity of catalyst could be enhanced by adding assistant electrocatalysts, the 4A-zeolite as assistant electrocatalyst was doped into Pt/C catalyst by simple mixing. The corresponding electrocatalytic activity for electrooxidation of methanol was evaluated in alkaline medium by several electrochemical techniques, including cyclic voltammetry, electrochemical impedance spectroscopy and chronoamperometry. It was shown that the electrocatalytic activity of the 4A-zeolite modified Pt/C catalyst was much better than that of the Pt/C catalyst. The increased electrocatalytic activity could be attributed to that the advanced properties of the micrometer 4A-zeolite with nano-porosity could significantly increase the effective electrode surface and facilitate the diffusion of analytes into the film of electrode surface.
Carbonized bacterial cellulose based carbon paste electrode (BCPE) was fabricated with nano-dimension carbonized bacterial cellulose (BC) fiber and studied by SEM, cyclic voltammetry and electrochemical impedance spectroscopy. Compared with traditional carbon paste electrode (CPE), a faster electron-transfer kinetics process happened on BCPE in wide scan rate ranges. Moreover, PMo12 was successfully assembled on BCPE surface by cyclic voltametric scanning method. Good stability and catalytic activity to the reduction of nitrite were observed on PMo12/BCPE. This novel carbonaceous materials is prospected to be used in electrocatalysis and other fields due to its mentioned advantages.
引文
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