臺灣博碩士論文加值系統

資源化矽泥廢料已成為晶圓生產國內重要的減廢政策，由於廢料中含有大量的矽屑、碳化矽、切割液與金屬雜質等，其中無論矽屑、碳化矽或切割液均可再利用，有效資源化矽泥廢料與創新回收物應用端，有助於提升晶圓製造系統的循環經濟價值。
本研究首先探討以沉降或離心法回收切割液的可行性並分析溶劑添加對切割液回收品質的影響。於矽與碳化矽定量上，文中探討了數種技術於分析矽與碳化矽組成上的差異。再者，研究以酸處理法去除矽泥廢料中的金屬雜質，包括酸的種類、濃度與固液比等，以及其反應動力學形態均有詳盡的分析。此外，本研究以垂直式沉降槽來進行廢料中的固體分選，並探討理論計算與實際沉降間的差異。另外，研究探討矽屑作為氫能源的潛力，以及矽與水反應生成的矽酸鹽應用。首先，在矽屑產氫上，論文中探討了矽粒徑、反應溫度與鹼液濃度對產氫的影響，並提出了一矽屑產氫的反應動力學機構。再者，將矽與水反應後的矽酸鹽溶液製備成吸附劑，其可有效去除鍍鎳廢水中的鎳離子，且吸附過程符合Langmuir model和擬二階動力模式。另一方面，矽酸鹽溶液改以硫酸滴定可製成膠態電解質，並可應用於鉛的氧化還原反應進行。
本論文涵蓋了目前資源化矽泥廢料的定量分析方法、固液分離、固體分選以及金屬溶除等技術，加上探討了能大量使用矽屑的應用端-矽產氫，以及針對矽產氫後的矽酸鹽進行高值化應用。經本研究的固液分離步驟後，高品質切割液可回收；經酸處理後，金屬雜質可溶除。剩下的固體可經沉降分離出富矽或富碳化矽粉；回收矽可直接反應產氫，矽酸鹽亦可再利用，最後留下高純度的碳化矽。簡單、低成本的資源化流程與策略有助於增加業者的投入意願，相信本論文已為矽泥廢料的分析、減量、再利用與零排放方向作了貢獻。

In a country producing silicon wafer, an important policy of waste reduction is to recycle the resource from silicon ingot sawing waste. In addition to metals impurities, a large amount of reusable Si, SiC and glycol solution are found in the sawing waste. Effective recycling of silicon sawing waste and innovative applications must improve the circular economic value of the wafer manufacturing system.
First of all, this study adopted gravity settling or centrifugation to recover glycol solution and analyzed the feasibility of recycling technologies. The experimental results show that adding different solvents is related to the quality of final recycled glycol solution. In quantification of Si and SiC, several ways to describe the composition of Si and SiC were compared. In addition, acid treatment was applied to remove metal impurities from silicon sawing waste. The effects of acidic species, concentration and ratio of solid to liquid on Fe dissolution and the dissolution kinetics were investigated. Moreover, the vertical sedimentation system was utilized to separate Si and SiC. The difference between the experimental results and theoretical calculation was discussed.
Furthermore, an idea about the potential of hydrogen energy generation from silicon and the applications of silicate produced from Si-water reaction were presented. First, the influence of particle size, alkali solution concentration, and reaction temperature were studied and its kinetic mechanism for Si-water reaction was proposed. On the one hand, the silicate solution was used to prepare an adsorbent and to remove nickel ions from wastewater. Analysis of experimental data indicated that the pseudo-second order kinetics and Langmuir model could well describe the adsorption process. On the other hand, the silicate solution was used to prepare gelled electrolytes by sulfuric acid titrating and to apply on the lead redox reaction.
In summary, this study are included that the Si and SiC quantitation, techniques regarding solid-liquid, solid-solid separation, metal removal, hydrogen production from silicon and applications of silicate solution. After solid-liquid separation, high-quality glycol solution was obtained; the metal impurities can be dissolved and removed by acids. Using sedimentation, the Si-rich or SiC-rich powders were obtained. The recovered Si could apply to hydrogen evolution, and then the silicate solution or high-purity SiC were reused. Simple, low-cost recycling processes and strategies encourage companies to adopt them and this study benefits the analysis, reduction, reuse and zero-emission of silicon sawing waste.

中文摘要 i
英文摘要 iii
誌 謝 v
目錄 vi
圖目錄 ix
表目錄 xvii
第 1 章 緒論 1
1-1 矽晶切割製程及其線鋸廢料 1
1-2 資源化矽泥廢料的重要性 3
1-3 氫能源 5
1-4 矽化合物製造與其應用 11
1-5 研究動機 15
第 2 章 文獻回顧 17
2-1 磨料回用與失效 19
2-2 切割液處理與金屬移除相關研究 19
2-3 矽與碳化矽分離之研究 26
2-4 回收矽或碳化矽之應用 48
第 3 章 自矽泥廢料回收切割液 52
3-1 實驗藥品與儀器 52
3-2 實驗方法 53
3-2-1 基本特性分析 53
3-2-2 沉降分離程序 56
3-2-3 離心分離程序 57
3-2-4 切割液除水 59
3-3 結果與討論 59
3-3-1 切割液與矽泥的性質分析 59
3-3-2 自矽泥回收切割液 61
3-3-3 添加劑對矽泥離心的影響 66
3-3-4 回收切割液純化 72
3-4 結論 74
第 4 章 矽泥廢料特性與定量技術研究 75
4-1 實驗藥品與儀器 75
4-2 實驗方法 76
4-2-1 矽泥特性分析 76
4-2-2 矽與碳化矽含量分析 78
4-3 結果與討論 79
4-3-1 矽泥廢料物性研究 79
4-3-2 矽與碳化矽的定量技術 83
4-4 結論 94
第 5 章 酸處理法去除金屬與其動力學分析 96
5-1 實驗藥品與儀器 96
5-2 實驗方法 97
5-2-1 建構Eh-pH關係圖 97
5-2-2 酸處理程序 101
5-2-3 極化曲線測量 101
5-2-4 傅里葉轉換紅外光譜分析 101
5-3 結果與討論 102
5-3-1 酸處理法去除矽泥廢料中金屬雜質 102
5-3-2 酸處理法去除鐵過程動力學研究 112
5-4 結論 115
第 6 章 矽與碳化矽分離 116
6-1 實驗藥品與儀器 116
6-2 實驗方法 117
6-2-1 矽泥廢料物性分析 117
6-2-2 分離槽設計 118
6-2-3 分離程序 118
6-2-4 固含量對分離的影響 119
6-2-5 磁場對分離的影響 119
6-2-6 電場對分離的影響 119
6-3 結果與討論 120
6-3-1 粒子沉降運動 120
6-3-2 固含量的影響 123
6-3-3 電場對分離的影響 126
6-3-4 磁力對矽泥中金屬移除的影響 128
6-4 結論 130
第 7 章 矽微粒產氫的反應機制 131
7-1 實驗藥品與儀器 131
7-2 實驗方法 132
7-2-1 矽微粒產氫實驗 132
7-2-2 氫氣定量方法 134
7-2-3 矽微粒表面氧化分析 137
7-2-4 矽微粒的粒徑分佈 137
7-2-5 多晶矽片氧化實驗 138
7-3 結果與討論 138
7-3-1 矽粒徑對產氫反應的影響 138
7-3-2 回收矽粉產氫之特性 147
7-3-3 化學反應程序 153
7-4 結論 157
第 8 章 矽微粒合成吸附劑及其吸附特性 158
8-1 實驗藥品與儀器 158
8-2 實驗方法 159
8-2-1 矽微粒合成吸附劑 159
8-2-2 合成粉體的性質分析 160
8-2-3 吸附金屬離子實驗 161
8-2-4 鎳廢液吸附實驗 162
8-3 結果與討論 163
8-3-1 合成吸附劑結構與吸附特性 163
8-3-2 合成吸附劑處理含鎳廢水 170
8-3-3 鎳離子吸附之動力學機制 172
8-3-4 鎳離子的吸附特性 174
8-3-5 不同吸附劑處理實廠廢水 176
8-4 結論 177
第 9 章 矽微粒製備膠態電解質 178
9-1 實驗藥品與儀器 178
9-2 實驗方法 179
9-2-1 矽微粒製備膠體電解質 179
9-2-2 矽凝膠分析 179
9-2-3 鉛電極在膠態電解質中性能測試 181
9-3 結果與討論 182
9-4 結論 194
第 10 章 總結 195
參考文獻 197
符號彙編 219

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