臺灣博碩士論文加值系統

傳統矽穿孔 (Through silicon vias, TSVs)製程屬於乾式製程，主要藉由離子蝕刻出矽穿孔，並乾式沉積二氧化矽絕緣層，再以物理氣相沉積 (Physical vapor deposition, PVD)或化學氣相沉積法 (Chemical vapor deposition, CVD)，沉積出氮化鈦 (TiN) 阻障層與銅晶種層，最後以濕式電鍍法填充金屬銅於矽穿孔中。近年發現，金屬銅與矽基材之間，經熱信賴度測試後，因兩者熱膨脹係數差異甚大，在銅、矽介面會產生相當大的熱機械應力 (Thermo-Mechanical Stress)，故在金屬銅與矽基材之間產生大量的破裂現象。因此，本研究嘗試使用熱膨脹係數較接近矽基材、具金屬擴散阻障能力且導電性極佳的石墨烯材料，取代傳統矽穿孔製程中的氮化鈦阻障層與銅晶種層，達到降低成本及簡化製程的目的，並利用濕式電鍍法於石墨烯上沉積鈷鎢 (CoW)合金與純鈷來取代原製程的金屬銅，鈷金屬具備比銅更低的熱膨脹係數及較長的電遷移壽命 (Electromigration life time)。
本研究主要探討基礎鍍液、電鍍添加劑、電鍍參數對填孔行為之影響與熱信賴度測試，其中，電化學分析部分以線性掃描伏安法 (Linear sweep voltammertry, LSV)探討電鍍添加劑的電化學行為，藉由電化學分析結果解釋不同分子量之抑制劑搭配單一平整劑之電鍍配方，並將其對應電鍍填孔之表現，發現電鍍配方對金屬離子還原反應的強抑制性及減少氫氣的庫倫量之行為，能達成鈷鎢合金與純鈷之超級填充。熱信賴度測試方面，本研究將填充鈷鎢合金與純鈷之TSVs於500℃的條件下，進行四小時熱信賴度測試，並於測試後利用光學顯微鏡、電子顯微鏡觀察鈷鎢合金或純鈷與矽基材介面之結構，證實熱膨脹係數較低的鈷鎢合金或純鈷搭配具金屬擴散阻障功能的石墨烯，便能有效解決TSVs製程於熱信賴度上的各種疑慮，因此，本研究所開發出的鈷鎢合金/石墨烯/矽穿孔製程與純鈷/石墨烯/矽穿孔製程，若能將其實行於工業量產，將是三維積體電路堆疊之矽穿孔製程技術的一大突破。

Usually, TSV fabrication uses a dry process, including via formation by reactive ion etching, SiO2 isolation liner deposition, TiN barrier layer and copper seed layer by chemical vapor deposition (CVD) or physical vapor deposition (PVD) formation and via filling with electrodeposited copper. Recently, industry and academic field find out that the difference of coefficient of thermal expansion (CTE) between the filled copper and silicon substrates often leads to failures in the TSVs interconnects because the CTE of copper is much higher than that of silicon. The filled materials in the TSVs with high CTEs will induce large thermo-mechanical stress at the interfaces between the filled materials and silicon substrates. To overcome this problem, graphene is selected to substitute the TiN barrier layer and the copper seed layer, which simultaneously reduces the cost and simplifies the original process. Since the CTE of graphene is closer to that of silicon. Moreover, we select cobalt, which possesses not only a lower CTE but also a longer electromigration lifetime than that of copper, as the filled material of TSVs.
In this work, the effects of electroplating baths, electroplating additives, electroplating operating parameters, filling performance and thermal reliability performance of the electrodeposited CoW alloy and pure Co are investigated. Linear sweep voltammetry (LSV) is carried out to electrochemically analyze these electroplating additives. The electrochemical behaviors of these electroplating additives are explored to explain the correlation between the suppression and the corresponding filling performance. The results indicate that the combination of suppressors with different molecular weights and a leveler can exhibit strong suppression and lead to CoW and pure Co bottom-up filling of TSVs. The thermal reliability examinations are also conducted at 500℃ for 4 hours. Then, the structure at the interface between the CoW alloy or pure Co and the silicon substrate is observed by optical microscope and scanning electron microscope. The results demonstrate that the combination of CoW or pure Co possessing a low CTE and graphene possessing excellent conductivity and barrier function can solve the thermal reliability problem in TSVs fabrication process.

摘要 i
Abstract ii
目錄 iii
圖目錄 vi
第 1 章、 緒論 1
第 2 章、 電化學理論及文獻回顧 2
第2.1節、 電化學理論 2
第2.1.1項、 電鍍原理及方法 2
第2.1.2項、 電化學反應程序 4
第2.1.3項、 極化與過電位 6
第2.1.4項、 電子轉移控制與質傳之關係 7
第2.1.5項、 電化學分析方法 9
第2.2節、 半導體製程技術發展與演進 10
第2.2.1項、 鋁製程技術缺失 10
第2.2.2項、 大馬士革雙鑲嵌技術 (Dual-Damscence) 10
第2.2.3項、 銅製程技術之矽晶圓阻障層材料 12
第2.2.4項、 銅製程技術缺失 14
第2.2.5項、 未來取代銅製程之替代方案 18
第2.3節、 矽穿孔製程 (Through Silicon Vias, TSVs) 22
第2.4節、 石墨烯 (Graphene) 23
第2.4.1項、 氧化石墨烯與還原氧化石墨烯 25
第2.5節、 氧化石墨烯的還原 27
第2.5.1項、 化學還原法 27
第2.5.2項、 氮摻雜還原法 28
第2.6節、 石墨烯化學接枝法 30
第2.7節、 鈷鎢電鍍基本鍍液 33
第2.7.1項、 氯離子系統、硫酸根系統、氨基磺酸根系統比較 33
第2.7.2項、 鎢酸根離子 34
第2.7.3項、 緩衝劑 34
第2.7.4項、 螯合劑 35
第2.8節、 鈷鎢與純鈷電鍍添加劑 37
第2.8.1項、 氯離子 37
第2.8.2項、 抑制劑 37
第2.8.3項、 平整劑 41
第2.8.4項、 光澤劑 43
第 3 章、 研究動機 46
第 4 章、 實驗藥品、裝置與步驟 48
第4.1節、 實驗藥品 48
第4.2節、 實驗裝置 49
第4.2.1項、 電鍍實驗系統 49
第4.2.2項、 電化學分析實驗系統 51
第4.3節、 儀器分析 53
第4.4節、 實驗步驟 61
第4.4.1項、 使用IGO (Improved Graphene Oxide)法合成氧化石墨烯水溶液 61
第4.4.2項、 還原氧化石墨烯接枝 62
第4.4.3項、 矽晶圓前處理 63
第4.4.4項、 哈林槽電鍍實驗 63
第4.4.5項、 電化學分析實驗 64
第 5 章、 實驗結果與討論 65
第5.1節、 硫酸鈷系統之鈷鎢合金填孔成效 65
第5.1.1項、 硫酸鈷系統之最佳抑制劑測試 65
第5.1.2項、 硫酸鈷系統孔底潤濕性探討 70
第5.1.3項、 比較硫酸鈷系統與氨基磺酸鈷系統之填孔行為 73
第5.2節、 氨基磺酸鈷系統之鈷鎢合金填孔成效 77
第5.2.1項、 氨基磺酸鈷系統之多段電流電鍍探討 77
第5.2.2項、 氨基磺酸鈷系統之最佳pH值與溫度判定 82
第5.2.3項、 氨基磺酸鈷系統之不同分子量PEG濃度探討 85
第5.2.4項、 氨基磺酸鈷系統之最適電流密度探討 90
第5.2.5項、 氨基磺酸鈷系統之硼酸效應 93
第5.3節、 探討鈷鎢合金填孔添加劑之電化學分析 99
第5.3.1項、 達成底部上移 (Buttom-up)之四劑電鍍配方分析 99
第5.3.2項、 超級填孔之三劑電鍍配方分析 103
第5.3.1項、 超級填孔於硼酸系統之四劑電鍍配方分析 106
第5.4節、 探討純鈷於TSVs電鍍填孔之成效 113
第5.4.1項、 純鈷系統之基礎鍍液探討 113
第5.4.2項、 不同分子量之聚乙二醇 (PEG)濃度探討 121
第5.4.3項、 純鈷系統之Leveler A最適濃度探討 124
第5.4.4項、 純鈷系統之兩段式電流電鍍探討 128
第5.4.5項、 探討Leveler A的濃度在TSV高深寬比 (AR 7)之成效 130
第5.5節、 石墨烯功能性之鑑定 132
第5.5.1項、 石墨烯均勻度之檢驗 132
第5.5.2項、 石墨烯接枝層厚度之檢驗 135
第5.5.3項、 石墨烯導電層之貢獻度鑑定 138
第5.5.4項、 石墨烯對銅阻障能力之功能性鑑定 139
第5.6節、 鈷鎢合金、純鈷與銅之熱信賴度測試與比較 141
第5.6.1項、 TSVs電鍍銅之熱信賴度測試 141
第5.6.2項、 TSVs電鍍鈷鎢合金之熱信賴度測試 144
第5.6.3項、 TSVs電鍍純鈷之熱信賴度測試 147
第5.6.4項、 TSV AR5~AR7電鍍之熱信賴度結果比較 149
第 6 章、 結論 152
第 7 章、 未來研究計劃 156
第 8 章、 參考文獻 157

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