依據(jù)實驗組前期對薄膜沉積的實驗徒恋,選擇-0.4mA進行兩電極的恒流沉積蚕断,并用橢偏儀進行在位監(jiān)測,每沉積180s后進行300nm到800nm的橢偏測試入挣。即在沉積180s亿乳、360s、540s径筏、720s葛假、900s、1080s后分別進行了橢偏儀全譜測試滋恬,測試角度為70°聊训。
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橢偏儀在位表征電化學沉積的系統(tǒng)搭建(二十二)- 沉積前裝置的橢偏數(shù)據(jù)
1形貌分析
圖4-2(a)是準在位監(jiān)測后沉積1080s時測試得到的SEM圖恢氯,在1μm放大倍數(shù)下看到沉積的薄膜顆粒大小不等(~10-103nm)带斑,形態(tài)上為不規(guī)則的塊狀。實驗組前期用三電極體系(Au/Si工作電極酿雪,Pt網(wǎng)對電極遏暴,Ag/AgCl參比電極)恒壓法(-0.05V)常溫下(T=20℃)沉積30分鐘得到的結(jié)果如圖4-2(b)所示。與恒壓沉積相比指黎,沉積薄膜粒徑不均勻性更強朋凉。
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(shù)據(jù)的分析
對沉積時間為180s、360s杂彭、540s、720s吓揪、900s亲怠、1080s的CU20薄膜分別進行了橢偏儀全譜(300-800nm)測試,獲得橢偏參數(shù)以及樣品整體的反射率和光學常數(shù)柠辞。
2.1沉積前裝置的橢偏數(shù)據(jù)
1团秽、Psi、Delta、α习勤、R實驗數(shù)據(jù)在-0.4mA時進行兩電極的恒流沉積踪栋,并在每沉積180s以后進行300nm到800nm的橢偏測試。在這個沉積電壓下图毕,不同時間沉積的庫侖量如表4-1所示夷都。由X-ray測試知該電流下沉積的為CU20,假設法拉第效率為100%予颤,則所對應的生長速率分別為0.94nm/s囤官,相應沉積時間下的CU20沉積厚度如表4-1所示。
如圖4-3(a)所示蛤虐,在沉積之前測試的Psi和Delta隨波長增加而增加党饮,在500nm處有躍遷,在長波段(600nm-800nm)存在波動笆焰。圖4-3(b)是對應的吸收系數(shù)α和反射率R值隨波長的變化圖劫谅,可以看到R值在500nm處存在躍遷,趨近于zui大值1后嚷掠,經(jīng)文獻查閱知這屬于基底Au的反射特性。說明沒有沉積之前所得到的橢偏測試結(jié)果主要反應的是襯底的信息荞驴,ITO和溶液對其影響甚小,也進一步證明該流動型裝置用于監(jiān)測薄膜沉積是可行的熊楼。對于α值霹娄,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(xù)可見光吸收光譜出現(xiàn)的峰位十分接近鲫骗,相對于文獻其峰位發(fā)生藍移且兩峰值存在差異犬耻,這可能是由于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(shù)
圖4-4(a)是沉積之前測試得到的n执泰、k隨波長的變化圖枕磁,從圖中可以看到短波段圖線較平滑,長波段數(shù)據(jù)波動大术吝。n值在500nm附近出現(xiàn)峰计济,k值在600nm附近出現(xiàn)峰。500nm處n值存在躍遷排苍,說明該處附近可能有等離子體共振峰的出現(xiàn)沦寂。
圖4-4(b)是沉積之前測試得到的、
淘衙,從圖中可以看到短波段數(shù)據(jù)曲線平滑传藏,長波段數(shù)據(jù)波動大。
、
均在500nm附近出現(xiàn)峰毯侦,這歸因于Au表面等離子體共振哭靖。
圖4-4 沉積0s時的n、k叫惊、款青、
隨波長的變化
經(jīng)過以上分析可知,在該體系下(ITO-溶液-Au/Si)霍狰,較短波段得到的橢偏參數(shù)比較光滑抡草,在較長波段得到橢偏數(shù)據(jù)波動比較大蔗坯。與較短波段相比長波段得到的數(shù)據(jù)誤差更小康震,該測試系統(tǒng)更適合較短波段測試。
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