椭偏仪在位表征电化学沉积的系统搭建（十五）- 弧形电解池的设计

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椭偏仪在位表征电化学沉积的系统搭建（十五）- 弧形电解池的设计

3.2弧形电解池

3.2.1池体样式

综合考虑椭偏仪的测量特点，初步设计了如图3-2(a)所示的池体模型图。可以看到该池体结构由两边的长方体和与之相连的半圆柱体及基底即工作电极载体构成。

池体的核心部分之一为中间的观察窗口，为了尽可能的减小椭偏仪的入射光在经过电解池池壁和溶液的损耗，则入射光必须垂直于池体壁入射；而椭偏仪的zui佳测量入射角在70°左右，是不固定的。综合考虑光的损耗及椭偏仪的测量特点，选择了半圆柱体作为观察窗口，这样就可以在既可以满足入射光垂直于池体壁入射又可以在一定范围内调节入射角度。

要使椭偏仪的出射光垂直入射后又经过一个对称的路径出射，则对基底工作面必须与半圆柱的圆面在同一平面，所以设计了如图3-2(d)所示的一个卡槽式载体，只要保证工作电极面和卡槽上表面齐平，当放置到半圆柱池底时就可满足要求。

两边的长方体设计一是为了使池体体积增大，增加电解质，便于电极的放置；二是这样设计可以使得电极在反应的过程中形成对称的物质传递路径。

3.2.2池体尺寸

中间的观察窗口半圆柱体的尺寸设计如3-2(c)所示，由于观察窗口工作时充满溶液，所以要考虑椭偏仪入射光在溶液中的光程，再结合后面电极的放置，设计了一个半径为15mm，池体壁厚为2mm的半圆体。在材料选取上，考虑到通常使用的椭偏仪入射波长是300nm到800nm波段，且要减小池体壁对光的损耗，所以观察窗口选用石英玻璃制作。两边长方体的尺寸设计如图3-2(b)所示，考虑的长度以及溶液的体积，长方体的长宽高分别为60mm、60mm及80mm。由于两边的池体设计主要起到增加溶液体积的作用，所以其制作材质没有特别的要求，这里选用5mm厚的亚克力板。

图3-2池体模型图及尺寸设计图

对于工作电极载体的设计如图3-2(d)所示，考虑到观察窗口的大小及电极的大小，其尺寸为20mm×55mm×5mm，材质选用5mm厚的亚克力板，这样当半圆柱体组装到两边的长方体后，把电极槽放到底面使得其上平面刚好是圆柱体的圆面，下底面刚好和长方体底面齐平。为了使电极放到电极槽后其工作面和其槽面平行，在长方体中间开凿一个长宽高分别为35mm、11mm、2mm的槽，这样电极就可以和观察窗口的圆柱圆面在同一个平面上，便于后续测试。

3.2.3电极的放置

如图3-3所示，红色部分为工作电极如图放到电极载体的卡槽里，有一部分在池体之外便于电极的连接；绿色部分为对电极，它平行于工作电极置于如图位置，后面实物用L型铂网电极；另外还有一个参比电极选用Ag/AgCl，图中没画出，用常见的毛细管靠近工作电极面。

图3-3电极放置图

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