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研究生: 張碩玲
Shuo-Ling, Chang
論文名稱: 荷載及退火溫度在矽單晶奈米壓痕行為及微觀結構變化上之效應分析
Effects of Load and Annealing Temperature on The Nanoindentation Behaviour and Microstructural Evolution of Single-Crystal Silicon
指導教授: 李偉賢
Lee, Woei-Shyan
學位類別: 碩士
Master
系所名稱: 工學院 - 機械工程學系
Department of Mechanical Engineering
論文出版年: 2009
畢業學年度: 97
語文別: 中文
論文頁數: 111
中文關鍵詞: 退火溫度矽單晶奈米壓痕
外文關鍵詞: Nanoindentation, Single-Crystal Silicon, Annealing Temperature
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  • 本研究主要是利用奈米壓痕的技術測量矽單晶的機械性質並探討奈米壓痕荷載及加熱溫度對其巨觀機械性質與壓痕影響區微觀之影響,透過所發展之定位陣列技術,可快速、準確且有效率的來搜尋微小奈米壓痕,並利用聚焦離子束顯微鏡切割出穿透式電子顯微鏡之觀測試片。首先,本實驗利用半導體製程於 (100) 方向之矽單晶分別先加熱至250℃、350℃、450℃,並持溫2分鐘,再分別進行30mN、50 mN、70mN的荷載,接著對未加熱的矽單經分別進行30 mN、40 mN、70 mN,藉此比較未加熱及不同加熱條件下,其微觀組織之變化及壓痕影響區之奈米結晶結構(nano-crystalline)與完全非結晶型(amorphous)結構混合結構形成之特徵與機制。
    巨觀機械性質的量測結果顯示,硬度(H)曲線與楊氏模數(E)曲線受壓痕尺寸效應、表面粗糙度(壓痕深度小於10 nm)所影響,楊氏模數約為178GPa,硬度值約為16GPa。從微觀結果顯示,矽單晶受奈米荷載及快速退火溫度之影響,造成壓痕器正下方之高應力塑性變形區的原子重新排列,單晶矽由原本的鑽石立方結構轉變為奈米結晶結構(nano-crystalline)與完全非結晶型(amorphous)結構混合結構。本研究發現,經過相同快速退火溫度後,荷載愈大時,壓痕影響區的底部產生愈多nano-crystalline與amorphous的混合結構;對未經過及經過250℃、350℃、450℃快速退火溫度後的矽單晶分別進行最大荷載為30 mN的奈米壓痕試驗,發現其壓痕影響區皆為amorphous結構;對未經過及經過250℃、350℃、450℃快速退火溫度後的矽單晶分別進行最大荷載為50 mN、70 mN的奈米壓痕試驗,發現其壓痕影響區為奈米結晶結構(nano-crystalline)與完全非結晶型(amorphous)結構混合結構,crystalline結構皆位在壓痕影響區底部,且隨著溫度的增加其分布的區域由底部逐漸往壓痕表面方向擴增。

    The study investigates the nano-mechanical properties of single-crystal silicon using a nanoindentation technique. The indented position is accurately identified using a proprietary position array system, and TEM specimens are extracted by the focused ion beam microscope technique quickly. The effects of indentation load and the annealing temperature on the microstructural evolution are also evaluated. The single-crystal silicon is annealed at the temperature of 250℃, 350℃, 450℃ for 2 min respectively,and then indented to the maximum load of 30 mN, 50mN, 50mN respectively.
    The overall tendencies of the hardness and Young’s modulus curves are governed by the indentation size effect and surface roughness for indentation depths of less than 10 nm, and by the substrate effect for indentation depths greater than 10% of the substrate. The hardness and Young’s modulus are measured about 16GPa and 178GPa respectively. The microstructural observations reveal that nanoindentation induces an atoms reorganization, and results in the formation of high-stress plastic deformation regions beneath the indenter. The microstructure of indentation affected zone of silicon substrate transfers from diamond cubic structure to mixed structure of nano-crystalline and amorphous.A complete amorphous phase within the indentation zone is produced at 30mN. However, in the specimens loaded at 40mN and 70mN, the microstructure of the indentation zone is characterized by a mixed structure comprising amorphous phase and nanocrystalline phase. The microstrucutral results also confirmed that the load-dependent nature of the unloading curves, namely pop-out events, is related to the different phase transformation mechanisms at various indentation loads.

    中文摘要 I ABSTRACT II 誌謝 III 目錄 IV 表目錄 VIII 圖目錄 IX 符號說明 XVIII 第一章 前 言 1 第二章 理論與文獻回顧 4 2-1奈米壓痕理論 4 2-1-1機械性質之量測 4 2-1-2初始卸載勁度與接觸面積之決定 6 2-1-3 連續勁度量測法(Continuous Stiffnes Measurement, CSM) 7 2-2 奈米壓痕實驗前的校正 9 2-2-1五點定位校正 9 2-2-2探針面積函數校正 9 2-2-3熱漂移校正 10 2-2-4機械性撓校正 11 2-2-5靜電力校正 11 2-3 影響量測之因素 12 2-3-1表面粗糙效應(Surface Roughness) 12 2-3-2擠出和沉陷效應(Pile-up & Sink-in Effect) 12 2-3-3壓痕尺寸效應(Indentation Size Effect, ISE) 13 2-4聚焦離子束顯微技術(Focused Ion Beam, FIB) 13 2-5 半導體矽單晶性質介紹 14 2-5-1矽單晶的簡介 14 2-5-2快速退火技術對於矽的應用 15 2-5-3奈米壓痕試驗對於矽的效應 15 2-5-4應力分布對於矽的影響 17 第三章 實驗方法與步驟 23 3-1實驗流程 23 3-2實驗儀器與設備 23 3-2-1電子束微影光罩製作系統(Electron Beam Lithography System, EBLS) 24 3-2-2奈米三維量測儀及奈米薄膜材料試驗機(Nano Indenter XP) 25 3-2-3快速退火爐(Rapid Thermal Annealing, RTA) 25 3-2-4聚焦式離子束顯微鏡(Focused Ion Beam, FIB) 25 3-2-5掃瞄式電子顯微(Scanning Electron Microscope, SEM) 26 3-2-6高解析穿透式電子顯微鏡(High Resolution Transmission Electron Microscope, TEM) 26 3-3試片製備 27 3-3-1 微影蝕刻製程 27 3-4實驗方法與步驟 28 3-4-1對試片進行不同條件的熱處理 28 3-4-2奈米壓痕試驗 28 3-4-3微觀結構的觀察 29 第四章 實驗結果與討論 41 4-1 矽晶圓機械性質之討論 41 4-1-1荷載-壓痕深度的曲線關係之分析 41 4-1-2楊氏模數-壓痕深度的曲線關係之分析 43 4-1-3硬度-壓痕深度的曲線關係之分析 45 4-2壓痕表面形貌之討論 46 4-3壓痕剖面形貌之討論 46 4-3-1 對未經快速退火處理前的矽單晶進行30mN、40mN、70mN荷載的奈米壓痕試驗之壓痕剖面形貌分析 47 4-3-2 對經250℃快速退火熱處理後的單晶矽進行30mN、50mN、70mN荷載的奈米壓痕試驗之壓痕剖面形貌分析 48 4-3-3對經350℃快速退火熱處理後的單晶矽進行30mN、50mN、70mN荷載的奈米壓痕試驗之壓痕剖面形貌分析 49 4-3-4對經450℃快速退火熱處理後的單晶矽進行30mN、50mN、70mN荷載的奈米壓痕試驗之壓痕剖面形貌分析 50 第五章 結論 102 六、參考文獻 104 自述 111

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