Central Department of Chemistry, Tribhuvan University, Kirtipur, Kathmandu, Nepal.
Talanta. 2010 Sep 15;82(4):1448-54. doi: 10.1016/j.talanta.2010.07.016. Epub 2010 Jul 16.
Polycrystalline silver sulphide/silver iodide ion selective electrodes (ISEs) with four different compositions, 9:1, 2:1, 1:1, 1:9 Ag(2)S-AgI mole ratios, have been fabricated in the laboratory and characterized by X-ray diffractometry (XRD), scanning electron microscopy (SEM), and electrochemical impedance spectroscopy (EIS). X-ray diffraction studies show the presence of Ag(3)SI, Ag(2)S and AgI crystalline phases in the electrode material. The electrode surfaces have been found to become smoother and lustrous with increasing percentage of silver sulphide in silver iodide. ISE 1:1, ISE 2:1 and ISE 9:1 all responded in Nernstian manner with slopes of about 60 mV/decade change in iodide ion concentration in the linear range of 1 x 10(-1) to 1 x 10(-6)M while ISE 1:9 showed sub-Nernstian behavior with slope of about 45 mV up to the concentration 1 x 10(-5)M. Two capacitive loops, one corresponding to the charge transfer process at metal electrode and the back contact and a second loop corresponding to the charge transfer process at membrane-electrolyte interface have been observed at high and low frequency ranges, respectively. Mott-Schottky analysis shows that the materials are n-type semiconductors with donor defect concentrations in the range of 5.1 x 10(14) to 2.4 x 10(19)/cm(3).
实验室制备了具有四种不同组成(9:1、2:1、1:1、1:9Ag(2)S-AgI 摩尔比)的多晶硫化银/碘化银离子选择性电极(ISE),并通过 X 射线衍射(XRD)、扫描电子显微镜(SEM)和电化学阻抗谱(EIS)进行了表征。X 射线衍射研究表明,电极材料中存在 Ag(3)SI、Ag(2)S 和 AgI 结晶相。随着碘化银中硫化银百分比的增加,电极表面变得更加光滑有光泽。ISE 1:1、ISE 2:1 和 ISE 9:1 均在碘离子浓度的线性范围 1 x 10(-1) 至 1 x 10(-6)M 内以 Nernst 方式响应,斜率约为 60 mV/decade 变化,而 ISE 1:9 则表现出亚 Nernst 行为,斜率约为 45 mV 直至浓度为 1 x 10(-5)M。在高、低频范围内分别观察到两个电容环,一个对应于金属电极和背接触的电荷转移过程,另一个对应于膜-电解质界面的电荷转移过程。Mott-Schottky 分析表明,这些材料是 n 型半导体,施主缺陷浓度在 5.1 x 10(14) 至 2.4 x 10(19)/cm(3) 范围内。