臺灣博碩士論文加值系統

近年來，碳化矽 (SiC)物件因其卓越的性能而在各個領域中備受青睞，如高溫穩定性、耐磨性、高硬度、高導熱性和抗腐蝕性等。隨著社會的不斷進步，工業和生活中的廢水排放問題日益嚴重，導致油水汙染問題日益突出。SiC薄膜因其在油水分離中的卓越表現而引起了廣泛關注，進而推動了對SiC製備技術的更深入研究和發展。然而，製備SiC物件通常需要超高溫的氣氛燒結系統（>1800℃ @ Ar）。此外，傳統陶瓷製程限制了成品幾合結構的設計發想，從而侷限了SiC製品的應用發展。因此，開發一個更為簡單且靈活的SiC製備技術成為當今SiC相關研究的重要課題之一。
本研究提出了一種結合3D列印和SiC/SiO2原位轉化機制的方法，以實現簡單製備SiC物件。首先，通過高溫氧化過程使SiC粒子的表面生成SiO2，有效降低SiC粒子的吸光度和折射率幫助列印。接著，將這些處理過的粒子與光敏性樹脂混合，形成光固化3D列印的SiC懸浮液。研究中我們使用數位光程序 (DLP)進行列印，製備薄膜生胚。接著，我們探討了不同的脫脂燒結程序對SiC/ SiO2原位轉化與燒結的影響。研究發現，在真空和氬氣保護下，將生胚中的樹脂進行碳化處理 (在200-600℃範圍內) ，並在真空下進行1530°C燒結程序。研究發現，此程序無法將SiO2成功還原回SiC，但能形成具結構強度的SiC/SiO2薄膜，且具有競爭力的水通量與良好的油水分離效能。接續我們改將列印胚體在氬氣中進行脫脂與燒結(1350°C-1600°C)，結果發現成功地使SiO2 與C進行還原反應，最終形成SiC物件。
本研究驗證了SiC表面氧化生成SiO2可提升SiC的可印性，成功列印出SiC胚體。而在後續的脫脂燒結過程中，驗證了SiO2殼層確實可成功與碳化樹脂反應還原成SiC，得到純SiC成品。雖然目前最終的SiC列印成品尚未能具有足夠的機械強度進行薄膜應用，但本研究已為我國SiC陶瓷3D列印技術發展立下一個新的里程碑。

In recent years, silicon carbide (SiC) objects have been highly favored in various fields due to their outstanding performance, such as high temperature stability, abrasion resistance, high hardness, high thermal conductivity, and corrosion resistance. With the continuous progress of society, the problem of wastewater discharge from industrial and domestic sources has become increasingly severe, leading to a growing concern over oil/water pollution issues. The excellent performance of SiC membranes in oil/water separation has garnered widespread attention, thereby promoting further in-depth research and development of SiC fabrication technology. However, the fabrication of SiC objects typically requires ultra-high-temperature atmosphere sintering systems (>1800℃ @ Ar). Furthermore, traditional ceramic fabrications limit the design and conception of complex structures, thus restricting the application development of SiC products. Therefore, developing a simpler and more flexible SiC fabrication technique has become one of the key topics in current SiC-related research.
This study proposes a method that combines 3D printing with the in-situ transformation mechanism of SiC/SiO2 to simplify the fabrication of SiC objects. Initially, the study employs an oxidation process to create SiO2 on the surface of SiC particles, effectively reducing the absorbance and refractive index of SiC particles to aid printing. These modified particles are then mixed with photosensitive resin to form a slurry for curable 3D printing of SiC. Using digital light processing (DLP), membrane precursors are printed. Furthermore, the influence of different debinding and sintering processes on the in-situ transformation and sintering of SiC/SiO2 is investigated. It is found that under vacuum and argon protection, resin in the membrane precursors undergoes carbonization treatment (within the range of 200-600℃) and a sintering process at 1530℃ in vacuum. This procedure fails to successfully reduce SiO2 back to SiC but yields SiC/SiO2 membranes with structural strength, competitive water flux, and effective oil/water separation performance. Subsequently, we revised the debinding and sintering of the membrane precursors in argon (1350℃-1600℃), successfully achieving the reduction reaction between SiO2 and C, ultimately forming SiC objects.
This study validates that the surface oxidation of SiC to generate SiO2 enhances the printability of SiC, successfully printing SiC membrane precursors. In the subsequent debinding and sintering process, it is confirmed that the SiO2 shell can indeed react with the carbonized resin to be reduced back to SiC, yielding pure SiC products. Although the current printed SiC membrane precursors do not yet possess sufficient mechanical strength for membrane applications, this study has set a new milestone for the development of SiC ceramic 3D printing technology in our country.

摘要 I
Abstract II
誌謝 IV
目錄 V
圖目錄 VII
表目錄 X
第1章 緒論 1
1-1前言 1
1-2研究方向 4
第2章 文獻回顧 5
2-1 碳化矽 5
2-1-1 碳化矽油水分離薄膜 6
2-2 3D列印 7
2-2-1 3D列印七大製程 9
2-2-2 陶瓷光固化列印 16
2-2-3 碳化矽光固化列印 19
2-3 碳熱還原反應 23
第3章 實驗 26
3-1實驗藥品 26
3-1-1陶瓷粉末材料 26
3-1-2光敏性樹脂成分 27
3-1-3 其他相關藥品 29
3-2實驗儀器 30
3-2-1 陶瓷製程之相關設備 30
3-2-2 特性分析相關儀器 34
3-3碳化矽薄膜製造流程 36
3-4 薄膜通透性測試 38
第4章 結果與討論 40
4-1 二氧化矽殼層助於列印之鑑定 40
4-2 SiC懸浮液配方 48
4-2-1 單體的選用 48
4-2-2 固含量 49
4-2-3 分散劑比例 50
4-3 燒結後薄膜之鑑定 52
4-3-1 真空中脫脂燒結 54
4-3-2 氬氣中脫脂燒結 57
第5章 結論 62
第6章 參考文獻 64

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