橢偏儀在位表征電化學(xué)沉積的系統(tǒng)搭建（三十二）- 總結(jié)與展望

正文

橢偏儀在位表征電化學(xué)沉積的系統(tǒng)搭建（三十二）- 總結(jié)與展望

上文主要用設(shè)計的微流腔體進(jìn)行了橢偏儀的在位監(jiān)測與分析锚贱。實驗包括三個部分，一是不同電流下Cu₂O膜的沉積关串；二是準(zhǔn)在位橢偏儀監(jiān)測Cu₂O薄膜的沉積過程拧廊，即每沉積180s后進(jìn)行300-800nm波段的橢偏儀測試，共測試了6組(180-1080s)晋修；三是實驗是橢偏儀在位監(jiān)測Cu₂O薄膜的沉積過程吧碾，0-1080s，橢偏儀取樣時間約為13s墓卦。經(jīng)過對實驗得到的橢偏譜分析擬合知：

1．對于該微流電解池體系倦春，用-0.4mA的恒流沉積可以得到單一的Cu₂O薄膜，故而后續(xù)實驗選-0.4mA作為沉積電流落剪；

2．準(zhǔn)在位橢偏儀監(jiān)測Cu₂O薄膜的沉積得到橢偏譜整沒有呈現(xiàn)出隨沉積時間的一致變化規(guī)律睁本，但是和0s比，由于Cu₂O薄膜的出現(xiàn)忠怖，R值變小了呢堰。擬合得到的厚度顯示沉積速率是隨著時間發(fā)生變化的，Cu₂O薄膜的生長方式可能是島狀和層狀生長相結(jié)合凡泣，其中單獨(dú)層狀生長擬合得到的庫倫轉(zhuǎn)換效率為36%枉疼，單獨(dú)島狀生長得到的庫倫轉(zhuǎn)換效率為50%皮假。

3．通過單波長實時在位監(jiān)測Cu₂O薄膜的沉積發(fā)現(xiàn)，用準(zhǔn)在位擬合得到的薄膜厚生長速率計算出的Psi和Delta值和實驗測試得到的值在數(shù)值和峰位上都有差別這可能與沉積過程的差異有關(guān)骂维。在準(zhǔn)在位全譜掃描中是每沉積180s后停下來進(jìn)行約17分鐘測橢偏測試钞翔，然后再重復(fù)測試到沉積時間為1080s，而單波長測試是不間斷沉積1080s席舍。所以可能由于沉積中間的間隔帶來薄膜表面的差異布轿，進(jìn)而影響得到薄膜的表面形貌。通過SEM對比發(fā)現(xiàn)来颤，連續(xù)沉積的1080s得到的Cu₂O薄膜表面島狀較明顯汰扭，這也是導(dǎo)致實驗和計算得到的Psi和Delta值不同的原因。

本文主要針對橢偏儀在位檢測薄膜沉積系統(tǒng)搭建福铅，并以Cu₂O薄膜的沉積為例進(jìn)行了實時在位監(jiān)測與分析萝毛。研究內(nèi)容包括了：（1）在位監(jiān)控裝置的設(shè)計。主要展開電解池的設(shè)計滑黔，包括用COMSOL進(jìn)行電場分布的擬合笆包，從而設(shè)計電極的位置等。并根據(jù)實驗和光路的調(diào)節(jié)的優(yōu)化制備了兩種類型的電解池略荡。（2）不同溶液濃度對實驗的影響庵佣。用Pb溶液為案例，進(jìn)行了不同濃度的Pb溶液的橢偏譜汛兜。（3）橢偏儀在位監(jiān)測Cu₂O薄膜的生長過程巴粪。研究包括全譜(300-800nm)橢偏儀Cu₂O薄膜沉積的準(zhǔn)在位監(jiān)測以及單波長(380nm)橢偏儀Cu2O薄膜沉積的在位監(jiān)測。主要結(jié)論包括：

（1）設(shè)計和制備了用于橢偏儀電化學(xué)在位測試的微流腔體電解池粥谬。

（2）利用微流腔體的電化學(xué)電解池肛根，用全譜橢偏儀在位監(jiān)測Cu₂O薄膜的沉積過程。利用光學(xué)模型的建立擬合橢偏譜得到了不同沉積時間下的薄膜光學(xué)常數(shù)漏策、介電常數(shù)及厚度派哲。從而得到層狀模型下平均沉積速率為0.40nm/s。另外也發(fā)現(xiàn)掺喻，時間較短范圍內(nèi)（<360s)芭届，Cu₂O的生長為非線性，更趨近于島狀生長巢寡，通過擬合得到其生長沉積速率為d＇=0.005t^0.72nm/s喉脖，平均庫倫效率為50%。

（3）橢偏儀單波長（380nm）實時監(jiān)控Cu₂O薄膜沉積：在同樣的沉積條件下實時監(jiān)控在Au基底上的Cu₂O薄膜沉積（0-1080s)抑月，采樣時間約為13s树叽。實驗發(fā)現(xiàn)Psi和Delta的實驗值與利用全波長厚度擬合得到橢偏參數(shù)有所差異。這個差異可能來源于用于全譜測試時的測試所用的生長時間谦絮，實際上忽略了生長層在沒有加電壓并進(jìn)行橢偏儀測試時（>17min）產(chǎn)生的變化题诵。SEM也發(fā)現(xiàn)兩種情況下（1080s）得到的Cu₂O薄膜的表面形貌不同洁仗。

本課題通過設(shè)計微流腔體電解池實現(xiàn)了橢偏儀在位監(jiān)測Cu₂O薄膜的電化學(xué)沉積過程。

通過本次的研究性锭，對型號為Ellip-SR-I的橢偏儀在位監(jiān)測電化學(xué)薄膜沉積進(jìn)行了擴(kuò)展赠潦，為其他類似的監(jiān)測提供案例。但是本課題研究中還存在一些待解決的問題：

（1）需進(jìn)一步設(shè)計全譜掃描和單波長掃描的測試條件草冈。

（2）提高全譜掃描的測試時間：通過采樣率或者減少波長范圍她奥。

（3）進(jìn)一步用光刻等技術(shù)制備微流腔體，更好的控制液流降低液流等造成的影響怎棱。

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