臺灣博碩士論文加值系統

中文摘要
本論文主要描述以下列兩種電漿與電化學沉積製程技術之發展過程與重要研究發現：(I)低k介電材料的電漿表面改質以生長“本質”介電性阻礙層之技術，(II)自我對準全程電化學製程生長銅金屬化與無電鍍擴散阻礙層之技術。第一部份(第4章)敘述旋轉塗佈沉積的混合有機矽氧烷聚合物(Hybrid Organic Siloxane Polymer, HOSP)低k介電薄膜在O2、H2與N2三種單一氣氛以及N2/H2混合電漿環境下的電物化性反應行為。籠狀Si-O、Si-CH3、Si-H與C-H低偏極化鍵結會遭受O2(或H2、抑或流量比例不適當之N2/H2)電漿的嚴重破壞，促使網狀Si-O鍵結過度交鏈，並導致介電常數(k值)上升與電絕緣性的衰退。但是，適當的調整N2/H2之(80% N2/20% H2)混合電漿激發功率及處理時間(50 W/6 min)不但不會破壞低k特徵鍵結及介電絕緣特性，而且可以產生表面鈍化的效果，以減低O2電漿對HOSP薄膜的損傷以及抑制銅原子之高溫擴散行為。X光吸收光譜、穿透式電子顯微鏡以及二次離子縱深等分析證實：最佳化的N2/H2混合電漿輔以適宜之電漿輸入功率/能量能生長厚度僅~15 nm之Si-N、C-N與O-N複合鍵結鈍化層。而使HOSP薄膜不虞置於(1)氧惡劣性電漿的環境、抑或(2)300℃/1 hr高溫處理，而能維持：(1)穩定之化學結構、(2)低介電常數及電絕緣特徵與(3)良好的銅擴散阻礙行為。
第二部分(第5章)介紹，一種在Si基介電材料(HOSP或SiO2)表面整合電漿與電化學技術所開發出有別於傳統的敏化/活化或置換/活化之晶種製程，並具有“自我對準”無電鍍生長超薄(~ 20 nm)Co基或Ni基金屬化阻礙層或銅薄膜的能力。X光吸收光譜(X-ray Absorption Spectroscopy)、穿透式電子顯微術(TEM)、原子力顯微術(AFM)與掠角X光繞射圖譜(GIXRD)一致證實：HOSP薄膜經電漿(O2或N2/H2)處理並浸漬於具少量H2O2的鹼性水溶液後，會形成親水性並具負電位的“圖案化”表面，因此具有吸附水溶液之金屬離子的能力；吸附之金屬離子(Co2+或Ni2+)經還原步驟後能形成密集(但不會團聚)分佈的金屬(Ni或Co)奈米微粒(2－4 nm)；這些超微催化微粒能促進超薄之Co基、Ni基二元/三元無電鍍阻礙層之生長。剛沉積之阻礙層薄膜是由~20 nm的類非晶質(Amorphous-like)柱狀晶粒所組成，故具有高達6000 �搟gΩ-cm的電阻率。但是經475℃至550℃熱處理1 hr後，Co-W-P薄膜之電阻率會因結晶化、晶粒成長、P之偏析以及Co2P的析出而劇降至僅為50－80 μΩ-cm。此外，全程電化學之自我對準技術所製作的MIS結構物(「Si/HOSP/Co-W-P(或Co-P)/Cu」)具有：(1)高介面平整性、(2)高附著性以及(3)高電性可靠度的特色，因此有簡化大馬士製程的發展潛力。量測不同熱處理後MIS結構之I-V曲線證實：無電鍍Co-P與Co-W-P薄膜皆有阻礙銅原子之高溫擴散行為，其中，又以Co-W-P的擴散阻礙效果最佳。這是因為摻雜耐火金屬W元素之Co-W-P薄膜可提高(1)熔點(或結晶轉變)溫度與(2)晶界填塞能力，而進一步強化對銅原子之高溫沿晶擴散的阻礙能力。

Abstract
This dissertation describes the development and important findings of the following two plasma-related electrochemical deposition techniques: (I) using plasma surface treatments to modify low-dielectric-constant (k) thin films and thus to grow in-situ “intrinsic” dielectric barriers; (II) presenting a “self-aligned”, all electrochemical plating process to grow electrolessly plated copper and metal barriers. Part I, described in chapter 4, illustrates the response of spin-coated hybrid organic siloxane polymer (HOSP) films, in terms of dielectric, physical and chemical property variations, under the treatments of plasma generated using O2, H2 or N2 single gas, or various N2/H2 mixtures. O2 (or H2) plasma could heavily disrupt the low polarized molecular units, such as cage-like Si-O, Si-CH3 and Si-H, and caused an over-crosslinking of the network-like Si-O, thus resulting in a serious decay of the dielectric constant and insulating capability of the HOSP films. However, adequately controlling the N2/H2 flow-rate ratio (80% N2/20% H2), in conjunction with an appropriate power/energy deposition (50 W/6 min), not only protects the films against O2 plasma damage, but also retards high-temperature diffusion of copper due to surface passivation. Results based on x-ray photoelectron and absorption spectroscopies (XPS & XAS) and transmission electron microscopy (TEM), along with depth-profiling secondary ion mass analysis (SIMS), indicated that the passivation was due to the formation of a carbide/nitride-based surface layer (~15 nm) that contained implanted nitrogen atoms of various chemical bonding states including Si-N, C-N and O-N. The improvement was proven by the facts that, despite of being heavily exposed to O2 plasma, such N2/H2 plasma pretreated films still exhibited (i) an extremely stable chemical structure, (ii) an unchanged dielectric constant and (iii) minimum levels of copper diffusion and biased leakage current.
Part II (see chapter 5) presents a self-aligned, electrochemically integrated seeding/plating approach that can be used to fabricate patterns of cobalt-based metallic barriers, such as Co-P or Co-W-P, and copper films selectively on silicon-based dielectric (HOSP and SiO2) films using electroless plating. After sequentially pre-treated appropriately by a gaseous plasma (O2 or H2/N2) and a basic aqueous solution that contained sufficient amounts of peroxide hydrogen (H2O2), the surface of the dielectric films was modified as hydrophilic and negatively charged to adsorb highly populated metal cational ions (e.g., Co2+ or Ni2+), which could be reduced to transform without aggregation into metallic (nickel or cobalt) precipitates of sizes �T 4 nm; These catalytic particles can initiate the deposition of ultra-thin (~ 20 nm) electrolessly plated Co- and Ni-based diffusion barriers. The as-deposited barriers, comprising ultrafine (3－5 nm) crystallites embedded in amorphous-like, 20-nm-sized grains, are highly resistive (6000 μΩ-cm), but become highly conductive (50－80 μΩ-cm) following optimal annealing at temperatures �d 470℃ because of crystallization, grain growth and precipitation of Co2P. The adhesion strength and effectiveness of the Co-W-P and Co-P barriers against copper’s diffusion/drift are quantified. Finally, the capacity of this self-aligned method to fabricate MIS capacitor patterns of barrier (Co-W-P and Co-P) and copper with high reliability and adhesion is established.

目 錄
第1章、前言 1
第2章、文獻回顧 4
2.1 銅金屬導線製程 5
2.1.1無電鍍基本原理 8
2.1.2 無電鍍製程特徵 9
2.1.3 無電鍍製程在積體電路之應用 12
2.2 低k介電材料製程 17
2.2.1 介電特徵 20
2.2.2 低k介電材料分類 23
2.2.3 低k介電材料沉積技術 27
2.3 銅/低k介電材料製程整合趨勢 29
2.3.1低k介電材料電漿鈍化技術 29
2.3.2 金屬性銅擴散阻礙層 34
第3章、實驗步驟 67
3.1實驗步驟 67
3.1.1 電漿表面處理研究步驟(註) 67
3.1.2自我對準無電鍍沉積研究步驟(註) 68
3.2 主要製程設備及原理簡介 70
3.2.1 旋轉塗佈沉積 70
3.2.2 電漿表面改質(Plasma Surface Modification) 71
3.2.3 無電鍍薄膜沉積 73
3.2.4 熱處理設備 74
3.3 主要分析儀器簡介 74
3.3.1 傅利業紅外線光譜分析儀(FTIR)【FTIR-8201, Shimadzu Scientific Instruments Co., JPN】 74
3.3.2 二次離子質譜分析儀(SIMS)【IMS-4f, Cameca, FR】 75
3.3.3 X光電子光譜(XPS)【ESCA210, Thermo Electron Co., USA】及XAS光譜 76
3.3.4 穿透式電子顯微鏡(TEM)【JEOL 1200EX II, JEOL, JPN/ Hitachi HF-2000, Hitachi, JPN】 77
3.3.5 X光繞射分析儀(XRD)【D/MAX2500, Rigaku Co., JPN】 77
3.3.6 原子力顯微鏡(AFM)【NanoScopeⅡ, Veeco Instruments Inc.(原Digital Instruments), USA】 78
3.3.7 四點探針(Four-point Probe)【S-301, Signatone Co., USA】 80
第4章、矽氧烷低k介電層薄膜之電漿表面處理行為 93
4.1 旋塗HOSP介電層薄膜之特性 93
4.1.1 HOSP溶膠-凝膠結構 93
4.1.2 HOSP介電層薄膜製程與結構 94
4.2 氧、氫與氮單一氣氛電漿處理 97
4.2.1氧電漿破壞行為評估 97
4.2.2 氫與氮單一電漿氣氛處理行為評估 99
4.3 氮/氫混合電漿處理 100
4.3.1鈍化行為評估 100
4.3.2 抗氧電漿破壞行為 103
4.3.3 電性行為 104
4.3.4銅之高溫擴散阻礙行為 106
4.3.5表面鈍化層分析 107
4.4 結論 109
第5章、自我對準全程電化學奈米級金屬化圖案製程研究 130
5.1 無電鍍奈米催化晶種技術與特徵 132
5.1.1基本原理 132
5.1.2奈米催化晶種之結構特徵 133
5.1.3 表面處理對奈米催化晶種吸附之影響 136
5.1.4 自行對準無電鍍積層薄膜 140
5.2 無電鍍Co-W-P擴散阻礙層生長與特性 140
5.2.1 電性與微結構 140
5.2.2 機械(附著)性質 146
5.3 Co-P與Co-W-P擴散阻礙行為評估 146
5.4 結論 148
第六章、總結 168
參考文獻 170
附錄一、溶膠-凝膠(Sol-gel)反應行為與低k介電材料發展趨勢 192
附錄二、化學氣相沉積(CVD)低k介電薄膜發展趨勢 198
個人簡歷 200
致謝 204

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