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研究生： 馮喬
Feng, Chiao
論文名稱： 三維列印聚醯亞胺/奈米纖維素混摻氣凝膠
3D Printing of Polyimide/Cellulose Nanocrystals Composite Aerogels
指導教授： 游聲盛
Yu, Sheng-Sheng
學位類別： 碩士
Master
系所名稱： 工學院 - 化學工程學系
Department of Chemical Engineering
論文出版年： 2021
畢業學年度： 109
語文別： 英文
論文頁數： 100
中文關鍵詞： 聚醯亞胺 、三維列印 、奈米纖維素 、混摻材料
外文關鍵詞： Polyimide, Cellulose Nanocrystals(CNCs), 3D printing, Nanocomposite
相關次數： 點閱：175  下載：0 
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    • 由於聚醯亞胺氣凝膠良好的化學與物理性質，如高孔隙率、低密度及絕佳的熱阻絕性等。這些性質，使聚醯亞胺氣凝膠被廣泛地應用於航空、汽車工業與各種絕熱應用。然而，製備聚醯亞胺氣凝膠仍受限於傳統的模具成形，不僅不利於製造複雜三維結構，更是一種費時花錢的做法。
    有鑑於此，我們製備了一種以水為溶劑、可進行三維列印的混摻墨水。此墨水中含有聚醯胺酸、三乙胺及奈米纖維素。透過混和三乙胺及聚醯胺酸，我們可得到水溶性的聚醯胺酸/三乙胺混和墨水。隨後，再加入奈米纖維素作為流變性質改良劑與強化劑去改善、增強墨水及最後產物性質。此墨水具剪切稀化的流變性質，十分適合以直接書寫法進行三維列印。我們更以直接書寫法列印出了幾個較為複雜的三維物件，包括台灣本島、金字塔與網格結構。進一步將這些物件進行冷凍乾燥及高溫閉環，便形成聚醯亞胺/奈米纖維素混摻氣凝膠。此氣凝膠不僅擁有極佳的形狀保真度、溶劑與熱穩定性，更展現出優秀的壓縮模數(高達15 MPa)與低縮水率(約20 %)。另外，在掃描電鏡圖中我們更發現了多層次的孔洞分布。我們推測此分布應該是來自於冷凍乾燥過程及熱閉環過程。總的而言，根據這些結果，我們提供了一條可靠且便捷的方法製備複雜形狀的聚醯亞胺氣凝膠。

    Polyimide (PI)-based aerogels have been widely applied to aviation, automobile industry, and thermal insulation because of their superior properties, such as ultrahigh porosity, low density, and excellent thermal insulating ability. However, the fabrication of PI aerogels is still restricted to the traditional molding process. It is not a cost-effective and efficient method to fabricate complex structures.
    Herein, we proposed a facile, water-based 3D printable ink consisted of polyamic acid (PAA), triethylamine (TEA), and cellulose nanocrystals (CNCs). By mixing TEA with PAA, a water-soluble PAA/TEA ink would form. We further used CNCs as a rheological modifier and a reinforcing agent to improve the desired properties of the ink and the final product. The ink showed a shear-thinning behavior suitable for direct ink writing (DIW) 3D printing method. Several objects with higher complexity were fabricated by DIW, such as a honeycomb structure, hollow grids, a pyramid and a model of Taiwan island.
    The printed objects then underwent lyophilization and thermal imidization processes to form PI/CNCs aerogels. The final product showed excellent shape fidelity, solvent and heat resistant abilities, compressive modulus and low shrinkage ratio up to 20 % in volume. Furthermore, the analysis from a scanning electron microscope revealed a hierarchical structure inside the aerogels. This multi-stage pore distribution might come from the freeze-drying process and the thermal treatment. Overall, these results showed a reliable, new approach to fabricate complex structures of PI aerogels.

    摘要 I Abstract II Acknowledgement IV List of Figures X List of schemes XV List of abbreviations XVI CHAPTER 1. Introduction 1 1.1 Polyimide 1 1.1.1 Brief introduction of polyimide 1 1.1.2 Typical synthesis methods of polyimides 2 1.1.3 Applications of polyimides 5 1.2 Aerogels 6 1.2.1 Brief introduction of aerogels 6 1.2.2 Typical synthesis and fabrication process of aerogel 7 1.2.3 Various applications of aerogels 11 1.3 Polyimide aerogels 13 1.4 3D printing methods 15 1.4.1 Introduction of 3D printing method 15 1.4.2 SLA method 17 1.4.3 DLP method 18 1.4.4 FDM method 19 1.4.5 DIW method 21 1.4.6 Other 3D printing methods 23 1.5 3D printing methods of polyimide polymer 26 1.5.1 Introduction of 3D printing polyimide polymer 26 1.5.2 UV-assisted DIW (UV-DIW) method 26 1.5.3 Heat-assisted DIW method 28 1.5.4 SLA method 31 1.5.5 DLP method 34 1.6 Cellulose nanocrystals (CNCs) 36 1.6.1 Introduction, basic properties and synthesizing process of CNCs 36 1.6.2 Various applications of CNCs 39 1.7 Objectives 41 CHAPTER 2. Experimental methods 43 2.1 Materials 43 2.2 Synthetic procedures of PMDA-ODA type polyamic acid solid 43 2.3 Preparation of PAA-TEA with CNC ink 44 2.4 3D printing test 45 2.5 Rheological test 45 2.6 Preparation of PI, CNCs and PI-CNC composite aerogels 46 2.7 Mechanical test 46 2.8 Solvent resistance test 47 2.9 Heat resistance test 47 2.10 Thermal conductivity (λ) test 47 2.11 Shrinkage ratio calculation 48 2.12 Bulk density calculation 48 2.13 Characterization 48 CHAPTER 3. The design of 3D-printable PAA-TEA with CNC ink 50 3.1 Rheological test 50 3.2 FT-IR analysis 53 3.3 Solid-state NMR analysis 55 3.4 TGA analysis 57 3.5 Shrinkage ratio analysis 59 3.6 CNC burnt-out analysis 62 3.7 SEM analysis 65 3.8 Bulk density analysis 69 3.9 Compression test 70 CHAPTER 4. Application of 3D-printed object 76 4.1 3D printing process 76 4.2 Solvent resistance test 78 4.3 Thermal insulation test 80 CHAPTER 5. Conclusion 83 REFERENCE 84

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