本研究目標以傅立葉紅外光譜與電噴灑式氣相電泳法為基礎，開發定量分析技術作為銅箔製程用硫醇添加劑與半導體製程用化學品中不純物粒子分析之應用。
第一部分的研究為定量銅箔製程所使用的微濃度化學添加劑，以優化製程。銅箔是一種高純度金屬銅的薄層，具有優異的導電性、延展性和耐腐蝕性，廣泛應用於電子領域。在銅電鍍溶液中添加含硫醇基 (-SH) 的化學添加劑 (如促進劑和抑制劑) 對於優化銅箔製程至關重要。而銅電鍍液存在大量離子和強酸環境等複雜因素，導致分析極具挑戰性，因此，精確地量化銅電鍍液中硫醇添加劑變得十分關鍵。在本研究中，以金奈米粒子 (AuNP) 作為吸附劑，利用分子吸附原理將硫醇添加劑 (抑制劑 – 硫醇基化聚乙二醇 (Poly (ethylene glycol) methyl ether thiol, PEG-SH) 及促進劑 – 3-硫醇基丙酸 (3-mercaptopropionic acid, MPA)) 於銅電鍍液中進行分離，以避免銅電鍍液的複雜環境，並於AuNP上形成硫醇分子膜，從而提高硫醇添加劑在分析上的訊號雜訊比。透過衰減全反射式傅立葉轉換紅外光譜儀 (ATR-FTIR) 對於AuNP上的硫醇分子層進行定量，以及利用電噴灑式氣相奈米粒子電移動度分析儀 (ES-DMA) 輔助ATR-FTIR之定量分析結果，以提升定量分析的準確性。首先，我們藉由ATR-FTIR與ES-DMA對於AuNP上的PEG-SH進行測量，找到優化定量分析的參數條件，在AuNP膠體原液體積500 µL與吸附反應時間1小時下，有很好的定量穩定性。接著，在固定此AuNP數量濃度與吸附反應時間，得到PEG-SH和MPA的Langmuir吸附等溫曲線，得知在飽和吸附點前為可定量的濃度範圍。結果指出，在此參數條件與定量濃度範圍下，隨著銅電鍍液中硫醇添加劑的濃度增加，AuNP表面的硫醇添加劑之特徵峰的IR吸收度訊號呈顯著線性增加，並得到PEG-SH濃度可檢測範圍為5 µM至100 µM，MPA濃度可檢測範圍則為10 µM至200 µM。我們成功分離並定量銅電鍍液中的硫醇添加劑，實現對於銅箔製程更精確的控制。
第二部分的研究為對半導體製程中所使用的化學品溶液進行不純物粒子分析，以降低半導體製程中矽晶圓上的粒子缺陷數目。粒子缺陷的發生主要是粒子殘留於晶圓表面，會直接影響晶圓產量和最終電子設備產品的品質，所以在化學品供應端及早發現粒子並進行抑制，以避免粒子進入後續的晶圓製造是一項非常關鍵之技術。因此我們希望建立一分析方法，期望能成功發現與定量化學品溶液中可能的外來粒子。由於此類化學品溶液含有多種配方成分 (e.g., 溶劑和溶質) 的因素，導致分析時會因配方成分訊號干擾以致難以監測到這些不純物粒子。因此本研究利用ES-DMA技術和改變稀釋倍率的方法來排除多成分化學品的訊號干擾，以期能監測到化學品中可能存在的不純物粒子。首先以電噴灑方式，藉由在高導電度下降低噴灑液滴的尺寸來提昇溶劑揮發度，以有效地除去化學品溶液中的溶劑和高揮發度溶質，氣溶膠相中將僅剩乾燥後的低揮發度溶質聚集所生成的粒子和可能存在的不純物粒子兩種粒徑分佈。接著藉由調控化學品溶液的稀釋倍率來分離出溶質粒徑，使得能測得不純物粒子的粒徑。結果指出，當稀釋倍率為10倍時，僅測得一個因溶質聚集所生成的粒子之粒徑分布，得知不純物粒子被大量的溶質包覆；當稀釋倍率增加至100倍時，產生的溶質聚集所生成的粒子的粒徑減小，開始能與不純物粒子的粒徑分離與個別分析；在稀釋倍率增加至2000倍時，溶質聚集所生成的粒子的粒徑大小低於偵測極限，將能呈現不純物粒子之單一粒徑分布，並可藉由計算不同化學品溶液中的不純物粒子含量，了解使用不同過濾器過濾之成效。我們成功運用此技術找到化學品溶液中可能存在的不純物粒子，並對其進行定量，來評估過濾器效果以管控化學品溶液品質，在化學品供應階段解決可能的污染來源，來降低矽晶圓上的粒子缺陷。

The first part of the work focuses on quantifying trace chemical additives used in the copper foil manufacturing process. Copper foil, a thin layer of high-purity metallic copper, having excellent conductivity, ductility, and corrosion resistance, is extensively applied in various electronic applications. Thiolated (SH-containing) chemical additives (i.e., accelerator and inhibitor) in copper electroplating solution are known to be critical for optimizing the copper foil manufacturing processes. Due to the high ionic strength and acidity of copper electroplating solution, proper and accurate characterization of the thiolated chemical additives is a critical concern. In this study, a facile, accurate approach is developed for quantitative characterization of thiolated additives in the copper electroplating solution. Firstly, gold nanoparticles (AuNPs) were employed as an adsorbent for separating the thiolated chemical additives, namely, poly (ethylene glycol) methyl ether thiol (PEG-SH) as inhibitor, and 3-mercaptopropionic acid (MPA) as accelerator from other interfering chemicals present in the copper electroplating solution. Subsequently, quantitative analysis of the AuNPs in the form of thin particle film was performed using attenuated total reflection Fourier-transform infrared spectroscopy. Electrospray-differential mobility analyzer was employed orthogonally for the quantitative analysis of the amount of thiolated additives adsorbed on AuNP. Interestingly, the results indicated that the detection concentration ranges of 5 μM–100 μM for PEG-SH and 10 μM–200 μM for MPA, respectively. Overall, this work demonstrates a successful separation and analysis methodology for the thiolated additives in copper electroplating solution which enables the precise control over the copper foil manufacturing process.
The second part of the work is the analysis of impurity particles in chemical solutions used in the semiconductor manufacturing process, with the aim of reducing the number of particle defects on wafers. The occurrence of particle defects, mainly due to particles remaining on the wafer surface, directly affects wafer yield and the quality of final products. Therefore, early detection and suppression of particles at the chemical supply end are crucial to prevent introduction into subsequent wafer manufacturing. We aim to establish a method to successfully detect and quantify potential foreign particles in chemical solutions. Due to the presence of multiple components in the chemical solutions (e.g., solvents and solutes), component signal interference makes it difficult to monitor these impurity particles. This study utilized ES-DMA and method of changing dilution factor to eliminate the effects of multi-component chemical solutions, with the goal of detecting possible impurity particles in the chemicals. Initially, electrospray was employed to enhance solvent evaporation by reducing droplet size under high electrical conductivity, effectively removing high volatility components from the chemical solution. Only low-volatility solutes and impurity particles remained in the aerosol phase, showing two distinct size distributions. Subsequently, by adjusting the dilution factor of the chemical solution, we can separate the solute particles, enabling the detection of impurity particles. The results indicated that at a dilution factor of 10, only a single particle size distribution generated by solute aggregation was detected, suggesting that impurity particles were encapsulated by the solute. When the dilution factor was increased to 100, the particle size of the solute aggregation decreased, allowing for the separation and individual analysis of impurity particle sizes. At a dilution factor of 2000, particle size of solute was below the detection limit, presenting a single size distribution of impurity particles. By calculating the concentration of impurity particles in chemical solution, we assessed the effectiveness of different filters in filtering chemical solutions, effectively reducing the content of impurity particles. We have successfully identified and quantified potential impurity particles in chemicals, resolving potential contamination sources at the chemical supply stage to reduce particle defects on silicon wafers.

摘 要 I
Abstract III
致謝 V
目錄 I
圖目錄 III
第一章 緒論 1
1-1銅箔製程 1
1-2 銅電鍍液的用途 2
1-3 銅電鍍液的添加劑 3
1-4 硫醇添加劑之定量分析及分離技術 4
1-5 半導體製程的晶圓缺陷 5
1-6 粒子缺陷偵測技術 7
1-7 研究目的與方法 8
第二章 實驗方法 11
2-1 實驗藥品 11
2-2樣品製備方式與分析技術 13
2-2.1 溶液之配置方法 13
2-2.2 AuNP表面吸附分子之分析方法 16
2-2.3定量銅電鍍製程用硫醇添加劑之實驗設計 18
2-2.4定量半導體製程用化學品中的不純物粒子之實驗設計 20
2-3 分析儀器 22
2-4 分析儀器原理及方法 23
2-4.1 衰減全反射式傅立葉轉換紅外光譜儀 (ATR-FTIR) 23
2-4.2 電噴灑式氣相奈米粒子電移動度分析儀 (ES-DMA) 26
2-4.3 氣溶膠粒子靜電收集器 (Electrostatic precipitator) 29
2-4.4 掃描式電子顯微鏡 (Scanning electron microscopy) 30
第三章 結果與討論 31
3-1 銅電鍍製程用硫醇添加劑之定量分析 31
3-1.1 ATR-FTIR分析之實驗條件 31
3-1.2 銅電鍍液中的單一硫醇添加劑之分析 39
3-1.3 銅電鍍溶中的兩種硫醇添加劑之分析 48
3-2 半導體製程用化學品中不純物粒子之定量分析 52
3-2.1 稀釋倍率之影響 52
3-2.2 不同樣品溶液中的不純物粒子濃度 56
第四章 結論 60
第五章 未來展望 62
參考文獻 64

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