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在十二烷基硫酸钠(SDS)的溶液中,超声辐射PdCl2溶液,制得了纳米Pd粒子,用XRD、TEM和低温氮吸附-脱附等进行了表征。采用滴涂法制得纳米Pd修饰玻碳电极(Pd/GCE),利用循环伏安法及线性扫描伏安法研究了甲醛在Pd/GCE上的电化学行为。结果表明,超声反应60 min时,得到晶面呈放射形结构的球形纳米Pd粒子,比表面积为33 m2/g,粒径分布较集中,在5 nm左右。Pd/GCE对甲醛具有良好的电催化氧化能力,甲醛的氧化峰电流与其浓度在3.3×10-4～2.7×10-2mol/L范围内呈现良好的线性关系,检出限为1.1×10-4mol/L(S/N=3)。该修饰电极具有良好的重现性。
In the solution of sodium dodecyl sulfate (SDS), PdCl2 solution was sonicated and nano-Pd particles were obtained. The nano-Pd particles were characterized by XRD, TEM and low temperature nitrogen adsorption-desorption. The Pd / GCE nanosized Pd-GCE was prepared by a dropping method. The electrochemical behavior of formaldehyde on Pd / GCE was investigated by cyclic voltammetry and linear sweep voltammetry. The results showed that the spherical Pd nanoparticles with radioactive crystal structure were obtained at 60 min after ultrasonic reaction. The specific surface area was 33 m2 / g. The particle size distribution was more concentrated at about 5 nm. Pd / GCE has good electrocatalytic activity for the oxidation of formaldehyde. The oxidation peak current of formaldehyde shows a good linear relationship with the concentration of 3.3 × 10-4 ~ 2.7 × 10-2mol / L with the detection limit of 1.1 × 10- 4 mol / L (S / N = 3). The modified electrode has good reproducibility.