橢偏儀在位表征電化學沉積的係統搭建（二十二）- 沉積前裝置的橢偏數據

正文

橢偏儀(yi) 在位表征電化學沉積的係統搭建（二十二）- 沉積前裝置的橢偏數據

1形貌分析

圖4-2(a)是準在位監測後沉積1080s時測試得到的SEM圖，在1μm放大倍數下看到沉積的薄膜顆粒大小不等（~10-10³nm），形態上為(wei) 不規則的塊狀。實驗組前期用三電極體(ti) 係(Au/Si工作電極，Pt網對電極，Ag/AgCl參比電極)恒壓法(-0.05V)常溫下(T=20℃)沉積30分鍾得到的結果如圖4-2(b)所示。與(yu) 恒壓沉積相比，沉積薄膜粒徑不均勻性更強。

圖4-2CU₂0薄膜的SEM圖：(a)沉積1080s(b)實驗組前期恒壓常溫沉積

2不同沉積時間橢偏數據的分析

對沉積時間為(wei) 180s、360s、540s、720s、900s、1080s的CU₂0薄膜分別進行了橢偏儀(yi) 全譜（300-800nm）測試，獲得橢偏參數以及樣品整體(ti) 的反射率和光學常數。

2.1沉積前裝置的橢偏數據

1、Psi、Delta、α、R實驗數據在-0.4mA時進行兩(liang) 電極的恒流沉積，並在每沉積180s以後進行300nm到800nm的橢偏測試。在這個(ge) 沉積電壓下，不同時間沉積的庫侖(lun) 量如表4-1所示。由X-ray測試知該電流下沉積的為(wei) CU₂0，假設法拉第效率為(wei) 100%，則所對應的生長速率分別為(wei) 0.94nm/s，相應沉積時間下的CU₂0沉積厚度如表4-1所示。

如圖4-3(a)所示，在沉積之前測試的Psi和Delta隨波長增加而增加，在500nm處有躍遷，在長波段(600nm-800nm)存在波動。圖4-3(b)是對應的吸收係數α和反射率R值隨波長的變化圖，可以看到R值在500nm處存在躍遷，趨近於(yu) zui大值1後，經文獻查閱知這屬於(yu) 基底Au的反射特性。說明沒有沉積之前所得到的橢偏測試結果主要反應的是襯底的信息，ITO和溶液對其影響甚小，也進一步證明該流動型裝置用於(yu) 監測薄膜沉積是可行的。對於(yu) α值，在370nm和600nm附近存在吸收峰，其和文獻中報道的ITO玻璃基板上Au納米膜的連續可見光吸收光譜出現的峰位十分接近，相對於(yu) 文獻其峰位發生藍移且兩(liang) 峰值存在差異，這可能是由於(yu) Au薄膜上溶液和ITO帶來的影響。

圖4-3 沉積0s時(a)Psi和Delta(b)R隨波長變化

2.2裝置對應的光學常數

圖4-4(a)是沉積之前測試得到的n、k隨波長的變化圖，從(cong) 圖中可以看到短波段圖線較平滑，長波段數據波動大。n值在500nm附近出現峰，k值在600nm附近出現峰。500nm處n值存在躍遷，說明該處附近可能有等離子體(ti) 共振峰的出現。

圖4-4(b)是沉積之前測試得到的、，從(cong) 圖中可以看到短波段數據曲線平滑，長波段數據波動大。、均在500nm附近出現峰，這歸因於(yu) Au表麵等離子體(ti) 共振。

圖4-4 沉積0s時的n、k、、隨波長的變化

經過以上分析可知，在該體(ti) 係下(ITO-溶液-Au/Si)，較短波段得到的橢偏參數比較光滑，在較長波段得到橢偏數據波動比較大。與(yu) 較短波段相比長波段得到的數據誤差更小，該測試係統更適合較短波段測試。

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