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材料研究学报  2014, Vol. 28 Issue (6): 413-419    DOI: 10.11901/1005.3093.2013.869
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纳米Pd的六角相液晶模板合成及对乙醇的电催化氧化*
王艳丽1(),谭德新2,陈森1,卞玲1
1. 安徽理工大学材料科学与工程学院 淮南 232001
2. 安徽理工大学化学工程学院 淮南 232001
Synthesis of Nano-Pd Particles in a Quaternary System with a Hexagonal Liquid Crystal as Template and Their Electrocatalytic Activity for Oxidation of Ethanol
Yanli WANG1,**(),Dexin TAN2,Sen CHEN1,Ling BIAN1
1. Institute of Materials Science and Engineering, Anhui University of Science and
Technology, Huainan 232001
2. Institute of Chemical Engineering, Anhui University of Science and Technology, Huainan 232001
引用本文:

王艳丽,谭德新,陈森,卞玲. 纳米Pd的六角相液晶模板合成及对乙醇的电催化氧化*[J]. 材料研究学报, 2014, 28(6): 413-419.
Yanli WANG, Dexin TAN, Sen CHEN, Ling BIAN. Synthesis of Nano-Pd Particles in a Quaternary System with a Hexagonal Liquid Crystal as Template and Their Electrocatalytic Activity for Oxidation of Ethanol[J]. Chinese Journal of Materials Research, 2014, 28(6): 413-419.

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摘要: 

构建盐水、环己烷、表面活性剂和助表面活性剂四元体系, 采用六角相液晶为模板在避光温和条件下将Pd2+还原制备出纳米Pd催化剂, 用偏光显微分析、XRD、TEM、选区电子衍射 (SAED)和HRTEM等手段对其进行表征, 研究了反应时间对纳米Pd微观形貌和尺寸的影响, 并用循环伏安法研究了纳米Pd修饰玻碳电极对乙醇的电催化活性。结果表明, 避光反应24 h后制备出呈规则形貌的纳米Pd材料, 平均粒径为(31±1) nm, 对乙醇有较高的电催化活性和抗中毒能力。

关键词 金属材料六角相乙醇电催化    
Abstract

Nano-Pd catalyst have been synthesized by slow reduction of Pd2+ in a quaternary system of brine-cyclohexane-surfactant-cosurfactant with a hexagonal lyotropic liquid crystal as template in a dark place under soft condition. Then the synthesized Pd nano-particles were characterized by optical microscopy、XRD、TEM、and HRTEM with selected area electron diffraction (SAED). The electrocatalytic properties of the nano-Pd modified glassy carbon electrode (Pd/GCE) for ethanol oxidation had been also investigated by cyclic voltammetry. The results show that the synthesized nano-Pd particles after reaction for 24 h show more or less the same shape with regular morphology with a mean size of (31±1) nm. This material exhibits the excellent electrocatalytic activity and anti-poisoning ability for the ethanol oxidation.

Key wordsmetallic materials    hexagonal mesophases    palladium    ethanol    electrocatalysis
收稿日期: 2013-11-19     
基金资助:* 国家自然科学基金51303005, 安徽省教育厅重点基金KJ2013A087、KJ2013A095和安徽理工大学博士启动基金资助项目。
图1  SDS/盐水/正戊醇/环己烷体系拟三元相图
图2  A1、A2、A3、A4和A5等五个样品的偏光纹理照片
图3  样品的小角XRD谱
图4  纳米Pd的XRD图
图5  纳米Pd颗粒在不同放大倍数的TEM和HRTEM照片(ED插图)
图6  不同反应时间时纳米Pd的TEM像
图7  乙醇在不同电极上的电催化氧化循环伏安曲线
Electrode Eonset/V jp/mAcm-2 jf/jb
PdI/GCE -0.50 0.13 1.5
PdII/GCE -0.53 0.15 1.85
PdIII/GCE -0.57 0.48 6.25
PdIV/GCE -0.66 1.55 15.6
表1  不同电极上循环伏安测试数据
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