橢偏儀在位表征電化學沉積的係統搭建（十三）- 形貌及成分

正文

橢偏儀(yi) 在位表征電化學沉積的係統搭建（十三）- 形貌及成分

2.5形貌及成分

2.5.1形貌分析

表征樣品的形貌常用的儀(yi) 器是掃描電子顯微鏡(SEM)，其原理是通過高能的電子束掃描樣品表麵激發出背散射電子、二次電子和X射線等信號，然後對接受到的信號進行放大並顯示成像，實現對樣品形貌等的監測。掃描電子微鏡顯具有操作簡單方便，得到的圖像清晰，zui大程度還原真實樣品形貌等優(you) 點。通過掃描電子顯微鏡觀察Cu₂O薄膜，得到其表麵形貌與(yu) 顆粒尺寸等信息，從(cong) 而對Cu₂O薄膜有更加直觀了解。

2.5.2成分分析

得到的樣品薄膜通過X射線衍射譜儀(yi) 掃描確定其成分。X射線是一種波長約為(wei) 20到0.06Å的電磁波，利用原子內(nei) 層的電子被高速運動的電子轟擊產(chan) 生躍遷光輻射，從(cong) 而產(chan) 生氣體(ti) 的電離、熒光物質的發光以及照相乳膠感光等。用電子束來轟擊金屬―靶‖材時將產(chan) 生X射線，通過衍射圖譜的分析，可以獲得其成分、內(nei) 部原子或者分子的結構和形態等信息。當X射線掃描晶體(ti) 物質時，X射線因晶格間距等效光柵的存在而發生光的散射和幹涉。幹涉效應使得X射線的散射強度增強或減弱，其中強度zui大的光被認為(wei) 是X射線衍射線。圖2-5是晶麵間距是d的n級反射圖示。在布拉格公式中：

d為(wei) 晶麵間距，θ為(wei) 布拉格角，λ為(wei) 入射波長。當入射光照射到晶麵上時會(hui) 發生輻射，且輻射部分將成為(wei) 球麵波同步傳(chuan) 播，其光程差是波長的整數倍。一部分入射光的偏轉角度是2θ，會(hui) 在衍射圖案中產(chan) 生反射點。通過已知波長X射線測量出的θ角，得到晶麵間距d，從(cong) 而可分解析出材料的內(nei) 部原子、或分子結構。由衍射峰的強度可得出晶體(ti) 結晶度，再利用謝樂(le) 公式(Scherrer)即能計算出晶粒平均尺寸。謝樂(le) 公式(Scherrer)：

式中K是Scherrer常數，如果β是衍射峰的半高寬，那麽(me) K=0.89，如果β是衍射峰的積分高寬，則K=1；D為(wei) 晶粒垂直於(yu) 晶麵方向的平均厚度(nm)；θ為(wei) 布拉格衍射角；λ為(wei) X射線波長，λ=0.154056nm。

圖2-5X射線的晶體(ti) 衍射圖

2.6實驗主要化學試劑及設備

本小節主要對涉及到的化學試劑進行陳述。

2.6.1主要化學試劑

本實驗所用的化學試劑如表2-1所示：

表2-1實驗主要化學試劑

2.6.2主要製備及表征設備

本實驗所用的主要製備及表征設備如表2-2所示：

表2-2主要製備及表征設備

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