臺灣博碩士論文加值系統

現今科技進步使半導體製程日新月異，技術節點隨之縮小，半導體元件奈米化，銅金屬製程由於其電子平均自由路徑較高，在連導線微縮下會產生電子散射，造成其電阻率急遽上升導致性能下降。為克服銅金屬在先進製程下所遇到的瓶頸，鈷金屬與釕金屬皆擁有較短的電子平均自由路徑，元件尺寸微縮下，鈷和釕在次世代半導體互連導線中成為具有潛力的替代材料。此外釕金屬具有低電阻率、高熔點、高抗氧化性，這些卓越的性質使釕金屬在互連導線應用上不需使用阻障層與襯墊層。本研究利用電化學原子層沉積製備鈷釕合金薄膜，克服元件逐漸小型化導致溝槽深寬比隨之增加的情況，改善傳統真空製程階梯覆蓋率不足的問題。
本實驗在TiSi2基板上使用低電位逐層沉積鈷原子層和釕原子層，透過控制不同沉積電位製備鈷釕合金薄膜。實驗首先以循環伏安法獲得鈷與釕溶液在TiSi2基板上的還原電位，透過電流密度-時間曲線得到薄膜總電荷並計算其覆蓋率和成核成長機制，從電流密度-時間的關係圖中求得擴散係數。使用掃描式電子顯微鏡 (Scanning Electron Microscope, SEM)、能量散射光譜儀 (Energy Dispersive Spectroscopy, EDS)、拉曼光譜儀 (Raman Spectra)、X-ray繞射儀 (X-ray Diffraction, XRD)、X射線光電子能譜儀 (X-ray Photoelectron Spectroscopy, XPS)、四點探針 (Four point probe, FPP) 進行薄膜表面形貌、成分、相結構、原子鍵結及電性等分析。
由實驗結果得知，在5 mM CoCl2溶液與1 mM RuCl3溶液中，UPD-Ru電位固定為-0.7 V，UPD-Co電位-1.0 V時以電化學原子層逐層沉積50個循環後，每個週期的鈷原子層沉積量是1.05 Monolayer (ML)，釕原子層沉積量是0.94 Monolayer (ML)，透過成核成長曲線得知UPD-Co與UPD-Ru成核機制皆為瞬時成核，此外薄膜具有良好的表面形貌，透過能量散射光譜儀可得該參數所得薄膜之鈷成分與釕成份比例約為1:1。由上述可得知UPD-Co電位-1.0 V與UPD-Ru電位-0.7 V所得之薄膜具有較佳薄膜性質。

Advancements in technology have led to rapid changes in semiconductor processes, resulting in the reduction of technological nodes and the miniaturization of semiconductor components. In copper metallurgy, the increasing electron scattering due to the shrinking of interconnects has led to a drastic rise in resistivity, thereby compromising performance. To overcome this bottleneck in advanced processes, cobalt, and ruthenium metals, which possess shorter electron mean free paths, have emerged as potential alternative materials in next-generation semiconductor interconnect. Additionally, ruthenium offers low resistivity, high melting point, and excellent oxidation resistance, eliminating the need for barrier and liner layers in interconnect applications.
This study employs electrochemical atomic layer deposition to prepare cobalt-ruthenium alloy thin films, addressing the challenges posed by the increasing aspect ratio of trenches as devices shrink, and improving upon the insufficient step coverage of traditional vacuum processes.
Using low-potential sequential deposition of cobalt and ruthenium atomic layers on TiSi2 substrates, the experiment controls different deposition potentials to fabricate cobalt-ruthenium alloy thin films. Initially, cyclic voltammetry is utilized to determine the reduction potentials of cobalt and ruthenium solutions on TiSi2 substrates, followed by obtaining total film charge through current density-time curves to calculate coverage and nucleation mechanisms. Diffusion coefficients are derived from current density-time relationships. Surface morphology, composition, phase structure, atomic bonding, and electrical properties are analyzed using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), Raman spectroscopy, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and four-point probe (FPP).
Experimental results reveal that, in 5 mM CoCl2 and 1 mM RuCl3 solutions, with a fixed UPD-Ru potential of -0.7 V and UPD-Co potential of -1.0 V, after electrochemical atomic layer deposition of 50 cycles, the cobalt atomic layer deposition is 1.05 Monolayer (ML) per cycle, while ruthenium deposition is 0.94 ML per cycle. Additionally, the thin films exhibit favorable surface morphology, with EDS indicating a cobalt-to-ruthenium ratio of approximately 1:1. These findings suggest that thin films obtained at UPD-Co -1.0 V and UPD-Ru -0.7 V exhibit superior properties.

摘要.............................................................................i
Abstract......................................................................iii
誌謝.............................................................................v
目錄...........................................................................vi
表目錄.........................................................................xii
圖目錄........................................................................xiii
第一章 緒論.....................................................................1
1.1 前言.....................................................................1
1.2 研究動機 ................................................................3
第二章 文獻回顧 ............................................................... 7
2.1 銅製程 ................................................................7
2.2 鈷製程 ................................................................8
2.3 介金屬化合物 (Intermetallic Compound) ................................9
2.4 物理氣相沉積 (Physical Vapor Deposition, PVD)...........................10
2.4.1 濺鍍系統 (Sputtering System)..............................................10
2.4.2 真空蒸鍍系統 (Vapor Evaporation System)...................................13
2.4.3 離子鍍系統 (Ion Plating System)...........................................13
2.5 電化學原子層沉積 (Electrochemical Atomic Layer Deposition, ECALD)........14
2.5.1 電化學原子層沉積初步概念...................................................14
2.5.2 低電位沉積 (Under Potential Deposition, UPD)..............................14
2.5.3 功函數 (Working Functon)..................................................16
2.6 電化學分析原理...........................................................17
2.6.1 參考電極 (Reference Electrode, RE)........................................17
2.6.2 工作電極 (Working Electrode, WE)..........................................18
2.6.3 輔助電極 (Auxiliary Electrode, AE) .......................................18
2.6.4 循環伏安法 (Cyclic Voltammetry, CV).......................................19
2.6.5 計時電流法 (Chrono Amperometry, CA).......................................20
2.7 電化學成核原理...........................................................20
2.7.1 電化學反應過程.............................................................20
2.7.2 電化學成核理論.............................................................22
2.7.3 影響電化學成核因素.........................................................25
2.8 鈷合金製程..............................................................26
2.8.1 磁控濺鍍製備鈷合金薄膜.....................................................26
2.8.2 電化學沉積鈷合金薄膜.......................................................28
2.9 EC-ALD文獻探討.........................................................31
第三章 實驗流程與儀器介紹.......................................................44
3.1 實驗材料....................................................... 44
3.1.1 濺鍍靶材..................................................................44
3.1.2 實驗基板......................................................... 44
3.1.3 製程氣體........................................................ 44
3.1.4 化學藥品........................................................ 45
3.2 實驗設備 ............................................................46
3.2.1 磁控濺鍍系統 (Magnetron Sputter System)................................46
3.2.2 熱處理系統 (Annealing system)................................46
3.2.3 電化學原子層沉積系統(Electrochemical Atomic Layer Deposition System, ECALD) 47
3.3 實驗流程 ................................47
3.3.1 基板清洗................................48
3.3.2 TiSi2基板製備................................48
3.3.3 溶液製備................................49
3.3.4 EC-ALD 實驗步驟設定................................50
3.3.5 鈷釕薄膜之熱穩定性................................51
3.4 分析儀器及原理................................51
3.4.1 表面輪廓儀 (α-step)................................51
3.4.2 四點探針 (Four-Point Probe, FPP)................................51
3.4.3 掃描式電子顯微鏡 (Scanning Electron Microscope, SEM)......................52
3.4.4 能量散射光譜儀 (Energy Dispersive Spectroscopy, EDS)......................53
3.4.5 場發射掃描式電子顯微鏡 Filed Emission Scanning Electron Microscope, FE-SEM) 53
3.4.6 X光繞射分析儀 (X-ray Diffraction, XRD)................................53
3.4.7 X光光電子能譜儀 (X-ray Photoelectron Spectroscopy, XPS)...................55
3.4.8 拉曼光譜儀 (Raman Spectra) ................................55
3.4.9 塔弗曲線 (Tafel curve)................................56
第四章 結果與討論................................66
4.1 TiSi2基板結構性質分析................................66
4.1.2 TiSi2薄膜結構之電阻率分析................................68
4.1.3 TiSi2薄膜結構之Raman分析................................68
4.1.4 TiSi2薄膜表面形貌分析................................68
4.2 沉積電位對於鈷釕合金薄膜電化學沉積之影響................................69
4.2.1 探討鈷溶液在TiSi2基板上CV................................69
4.2.2 探討釕溶液在TiSi2基板上CV................................70
4.3 調控低電位沉積製備Co(Ru)合金薄膜的沉積行為 ............................71
4.3.1 以低電位層狀沉積Co(Ru)合金薄膜之電流密度-時間變化曲線........................71
4.3.2 以低電位層狀沉積Co(Ru)合金薄膜之成核成長曲線................................78
4.4 調控不同低電位沉積電位對於Co(Ru)合金薄膜電化學沉積結構影響.................82
4.4.1 Co(Ru)合金薄膜之EDS成份分析................................82
4.4.2 Co(Ru)合金薄膜之XRD分析................................83
4.4.3 Co(Ru)合金薄膜之Raman分析................................84
4.4.4 Co(Ru)合金薄膜之XPS分析................................85
4.5 調控不同低電位沉積電位對於Co(Ru)合金薄膜之表面形貌分析.....................86
4.5.1 以低電位沉積Co(Ru)合金薄膜SEM分析................................86
4.5.2 以低電位沉積Co(Ru)合金薄膜FE-SEM分析................................87
4.6 調控不同低電位沉積電位製備Co(Ru)合金薄膜沉積與擴散行為特性.................88
4.6.1 以低電位層狀沉積Co(Ru)合金薄膜之電流瞬態曲線................................88
4.6.2 以低電位層狀沉積Co(Ru)合金薄膜之Cottrell曲線................................91
4.6.3 以低電位層狀沉積Co(Ru)合金薄膜之Tafel曲線分析............................94
4.7 探討不同低電位沉積電位製備Co(Ru)合金薄膜之熱穩定性........................95
4.7.1 退火後以低電位層狀沉積Co(Ru)合金薄膜之XRD分析........................95
4.7.2 退火後以低電位層狀沉積Co(Ru)合金薄膜之Raman分析........................97
4.7.3 退火後以低電位層狀沉積Co(Ru)合金薄膜之XPS分析........................97
4.7.4 退火後以低電位層狀沉積Co(Ru)合金薄膜之SEM分析........................99
4.7.5 退火後以低電位層狀沉積Co(Ru)合金薄膜之Tafel分析........................100
第五章 結論..................................................................157
參考文獻............................................................... 158

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