橢偏儀在位表征電化學沉積的係統搭建（十九）- 圓形微流腔體

正文

橢偏儀(yi) 在位表征電化學沉積的係統搭建（十九）- 圓形微流腔體(ti)

3.3微流腔體(ti)

由於(yu) 半弧形電解池存在的不足，所以進行了池體(ti) 的改進，得到圓形微腔體(ti) 以及進一步改進的流動長方形微腔體(ti) 。它們(men) 都有易於(yu) 拆卸更換電極、操作簡單等優(you) 點。

3.3.1圓形微腔

圖3-16是圓形微腔製作完成的實物圖以及在橢偏儀(yi) 測試中的放置示意圖。該池體(ti) 主要由基底即工作電極Au/Si、橡膠圈和上麵的打孔ITO即對電極組成，他們(men) 由上下亞(ya) 克力板即四角的螺絲(si) 固定壓緊。其中上麵的亞(ya) 克力板去掉了一塊留出觀察窗口，減小光在傳(chuan) 播過程中的損耗。ITO上打孔用於(yu) 溶液的注入。電極的連接由銅膠帶實現。

圖3-16(a)實物圖;(b)橢偏儀(yi) 測試中的放置圖

用該電解池進行了薄膜沉積，電解液為(wei) 0.02MCu(CH₃COO)₂，0.1MCH₃COONa。由於(yu) 是兩(liang) 電極體(ti) 係Au/Si為(wei) 工作電極，ITO或Pb絲(si) 為(wei) 對電極，所以選擇恒壓沉積。由實驗組之前做的研究，選擇-0.4mA的電流進行沉積20分鍾。沉積結果如圖3-17所示，(a)為(wei) 以TIO作為(wei) 對電極沉積結果，(b)為(wei) 用Pt絲(si) 作(腔體(ti) 的上端由ITO換為(wei) 石英玻璃)為(wei) 對電極沉積的結果。

可以看到以ITO作為(wei) 對電極時，ITO上會(hui) 產(chan) 生大量的氣泡，而且實驗觀察可知氣泡會(hui) 隨著沉積時間的增加而變多變大。這樣以ITO為(wei) 對電極在該情況下進行橢偏測試不可行，因為(wei) 氣泡的存在會(hui) 極大影響光的傳(chuan) 輸，使得測試得到的數據基底的信息很難提取。

鑒於(yu) 沉積過程中會(hui) 在ITO上出現氣泡，所以考慮用Pb絲(si) 環代替ITO，如圖3-17(b)。可以看到在Pb絲(si) 環周圍同樣有氣泡產(chan) 生，但中間部分沒有，所以該方法改進了ITO做對電極的不足，用於(yu) 橢偏儀(yi) 測量可行。

圖3-17不同對電極示意圖

上述圓形微腔體(ti) 改進是成功的，和圓弧形池體(ti) 對比它有電極更換容易、溶液層薄、密封性好等優(you) 點。但是該池體(ti) 也存在不足之處，如池體(ti) 氣泡始終存在、腔體(ti) 容納電解液少等。所以在該池體(ti) 基礎上進一步改進池體(ti) ，得到了長方體(ti) 流動微腔池體(ti) ，如下節詳述。

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