橢偏儀在位表征電化學沉積的系統(tǒng)搭建（六）- 在位監(jiān)測電化學沉積

正文

橢偏儀在位表征電化學沉積的系統(tǒng)搭建（六）- 在位監(jiān)測電化學沉積

2.3在位監(jiān)測電化學沉積

目前報道過的在位監(jiān)測手段主要有電化學在位拉曼光譜法畜伐、在位傅里葉紅外光譜儀法闲孤、石英晶振儀法烤礁、質(zhì)譜儀法、在位橢偏儀法肥照。

電化學在位拉曼光譜法脚仔，其原理是通過介質(zhì)分子對入射光發(fā)出頻率的有明顯變化的散射現(xiàn)象，用單色入射光（圓偏振光與線偏振光)來激發(fā)由電極電位控制的電極表面舆绎，然后測定出散射得到的光譜信號鲤脏，如頻率吕朵、強度及偏振性能變化與電極的電位或者電流強度的變化關(guān)系猎醇。

在位傅里葉紅外光譜儀法(FTIRS)是由Bewick等人在20世紀80年代早期首創(chuàng)的努溃。在位傅里葉變換紅外光譜儀可以獲取電極上中性和離子吸附物的分子信息硫嘶，以及參與電化學反應的溶液種類。大量的研究已將在位FTIRS由光滑的表面向粗糙的表面擴展梧税，由靜態(tài)條件向動態(tài)條件擴展沦疾，由水相系統(tǒng)向非水相系統(tǒng)擴展称近。利用在位FTIRS技術(shù)可以得到的電化學雙分子層等圖像信息，達到對電催化反應以及帶電界面過程更深刻的理解哮塞。

圖1-11兩種在位FTIRS電池設(shè)計圖

兩種在位FTIRS電池設(shè)計方法已經(jīng)被開發(fā)出來刨秆，以減少電解質(zhì)的強紅外吸收，即內(nèi)部和外部反射裝置，其原理圖如圖1-11所示家凯。該方法適用于多種電極材料缓醋，包括金屬單晶電極、納米材料電極肆饶、氧化物材料電極和碳材料電極改衩，并能同時測定電化學反應中吸附物和溶液的種類。在位FTIRS也采用衰減全反射(ATR)模式的內(nèi)反射結(jié)構(gòu)驯镊，在高折射率的紅外透明母棱鏡上沉積一層金屬薄膜作為工作電極葫督。由于紅外光束從電極背面(通過棱鏡)聚焦在界面上，然后檢測到反射輻射板惑，因此溶液層的厚度對入射橄镜、出射光的影響可避免，故而液層的厚度將不再受到限制冯乘。然而洽胶，這種內(nèi)部反射結(jié)構(gòu)的電極材料僅限于紅外窗口棱鏡上的一個薄膜(小于100nm)，僅限于濺射或化學沉積的少數(shù)金屬(Au裆馒、Pt姊氓、Pd等)。

石英晶振儀是一種非常靈敏的質(zhì)量天平喷好，可以測量單位面積內(nèi)質(zhì)量的毫微克水平變化。石英是一種壓電材料梗搅，通常通過金屬電極施加適當?shù)碾妷汉萄洌梢允蛊湟砸?guī)定的頻率振蕩。在電極表面添加或去除少量的質(zhì)量可以影響振蕩的頻率无切。這種頻率的變化可以實時監(jiān)測，以獲得電極表面發(fā)生的分子相互作用或反應的有用信息哆键，如薄膜生長掘托、氧化、腐蝕或衰減等籍嘹。因此可以把石英晶振儀作為工作電極襯底烫映，從而用于監(jiān)控薄膜生長過程中的薄膜厚度沼本。石英晶振儀能給出沉積的量的多少，但是無法給出生長的模式锭沟，因此通常用于配合其他的測試方法抽兆，如橢偏儀。

質(zhì)譜儀法是通過用電場族淮、磁場把運動的帶電荷原子辫红、分子和離子等粒子，按其比荷進行分離檢測的方法祝辣。不同帶電粒子其質(zhì)荷比不同，偏轉(zhuǎn)的時間也不同蝙斜，質(zhì)譜儀就可以將這些不同的時間名惩、位置等信息轉(zhuǎn)變成光學數(shù)據(jù)，通過質(zhì)譜圖呈現(xiàn)出來孕荠，這樣混合物中的各種成分就可以被解析觀察娩鹉。可以用于解構(gòu)在電化學過程中溶液的變化等稚伍。

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