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研究生:Nigus Maregu Demewoz
研究生(外文):Nigus Maregu Demewoz
論文名稱:低密度 PMMA 奈米泡材的製備和表徵
論文名稱(外文):Fabrication and Characterization of Low-Density PMMA Nanocellular Foam
指導教授:葉樹開
指導教授(外文):Shu-Kai Yeh
口試委員:林育君葉樹開賴森茂邱方遒童世煌
口試委員(外文):Yu-Chun LinShu-Kai YehSun-Mou LaiFang-Chyou ChiuShih-Huang Tung
口試日期:2022-01-25
學位類別:博士
校院名稱:國立臺灣科技大學
系所名稱:材料科學與工程系
學門:工程學門
學類:材料工程學類
論文種類:學術論文
論文出版年:2022
畢業學年度:110
語文別:英文
論文頁數:177
中文關鍵詞:米泡材PMMA 共混物黏彈性雙峰泡材低密度奈米泡材PMMA-TPU 摻混物成核效率
外文關鍵詞:Nanocellular foamPMMA blendsviscoelastic propertiesbimodal foamLow-density nanocellular foamPMMA-TPU blendnucleation efficiency
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摘要
由於其優異的性能,奈米泡材是一種有前景的新材料。本研究使用批式發泡來製造以 CO2 作為發泡劑的低密度奈米多孔泡材。低密度奈米多孔泡材是高性能隔熱的絕佳選擇。然而,製造低密度奈米多孔泡材非常具有挑戰性。降低奈米孔泡材密度的一種方法是引入微米泡孔並製造雙峰泡材結構。目前已知雙峰泡孔結構可提供獨特的物理特性並有助於降低相對密度。本研究提出了一種通過混合不同分子量的 PMMA 來創建雙峰微泡孔/奈米泡孔結構的簡單方法。將微型氣泡引入均勻的奈米孔結構可能是降低泡材密度的一種方法,並且可能不會影響某些特性。除了雙峰結構之外,還觀察到從超微孔結構到奈米孔結構的轉變,從閉孔結構到開孔結構。這些轉變可能與非纏結 PMMA 含量的弛豫時間和重量百分比有關。雙峰奈米孔或開孔結構的形成可以通過粘彈性特性,例如弛豫時間來預測。
降低奈米孔泡材密度的另一種方法是使用高效成核劑增加孔密度並降低支柱分數。在本研究中,將聚甲基丙烯酸甲酯 (PMMA) 與三種不同硬度的熱塑性聚氨酯 (TPU) 混合,以研究 TPU 對奈米孔結構和泡材密度的影響。 TPU 的黏度控制了共混物的奈米結構。將 2 wt% TPU 與 PMMA 混合產生了一個分散良好的體系,最小的 TPU 粒徑小於 100 nm。 CO2 吹製的奈米孔泡材具有新的花束狀結構,孔密度為 1016 cells/cm3。這些 TPU 奈米粒子的成和效率可高達 3674 倍。成核效率的意外增加可能是由於 TPU 顆粒分散良好。如此高的成核效率產生了開孔結構,其中支柱體積的比例降低並顯著降低了泡材密度。我們可以製造出相對密度小於 0.2 且平均孔徑小於 100 nm的奈米孔泡材。在 PMMA 中添加 2 wt% 的 TPU 可使相對密度降低 32.26%,從 0.31 到 0.18。
This thesis highlights the comprehensive study of low-density nanocellular foam. Because of its excellent properties, nanocellular foam is new promising material. This research uses solid-state batch foaming to create low-density nanocellular foam with CO2 as a blowing agent. Low-density nanocellular foam is an excellent choice for high-performance thermal insulation. However, creating low-density nanocellular foam is very challenging. One way to reduce the density of nanocellular foam is to introduce microcellular cells and create a bimodal foam structure. Because the bimodal cellular structure gives special physical properties and lowers relative density, this study proposes a simple method for creating a bimodal microcellular/nanocellular structure by blending PMMAs with varying molecular weights. Introducing microsized bubbles into homogeneous nanocellular structures could be one way to reduce foam density while retaining some properties. Behind the bimodal structure, a transition from an ultramicrocellular to a nanocellular structure was observed. The cell structure evolved from a closed-cell to an open-cell structure. These transitions may be related to the relaxation time and weight percentage of non-entangled PMMA content. These properties may be applied to predict the bimodal nanocellular or open-cell structure formation.
The other way to reduce the density of nanocellular foam is by increasing the cell density and lowering the strut fraction using highly efficient nucleating agents. In this study, poly(methyl methacrylate) (PMMA) was blended with thermoplastic polyurethanes (TPUs) of different hardnesses to study the impact of TPUs on the nanocellular structure and foam density. The viscosity of TPU controlled the nanostructure of the blend. Blending 2 wt% TPU with PMMA generated a well-dispersed system, with the smallest TPU particle size less than 100 nm. The CO2-blown nanocellular foam possessed a bouquet-like structure with a cell density of 1016 cells/cm3. These TPU nanoparticles provided an ultrahigh nucleation efficiency of 3674 times. The unexpected increase in nucleation efficiency could result from the well-dispersed TPU particles. Such a high nucleation efficiency created an open-cell structure with decreased strut fraction and significantly lowered the foam density. We can create a nanocellular foam with a relative density of less than 0.2 and an average cell size of less than 100. Adding 2 wt% of TPU to PMMA reduces the relative density by 32.26%, from 0.31 to 0.18.
摘要 i
Abstract ii
Acknowledgments iii
List of Contents iv
List of Figures viii
List of Tables xii
List of Abbreviations and Symbols xiii
Chapter-1 Introduction 1
1.1 Background of the Study 1
1.2 Motivation and Goals 7
1.3 Thesis Organization 7
Chapter- 2 Literature Review 8
2.1 Polymer Foam 8
2.2 Classification of polymer foam 8
2.3 Foaming process 11
2.3.1 Blowing Agent 12
2.4 Fabrication of Nanocellular foam 14
2.5 Phase separation 15
2.5.1 Nucleation 20
2.5.1.1 Homogenous Nucleation 22
2.5.1.2 Heterogeneous Nucleation 24
2.5.2 Spinodal Decomposition 30
2.6 Batch Foaming Process 32
2.7 Properties of Nanocellular Foam 35
2.7.1 Relative Density 35
2.7.2 Mechanical Properties 36
2.7.3 Thermal Conductivity 37
2.7.4 Transparency 40
2.8 Challenges in Nanocellular Foam 41
Chapter 3 Experimental Methods 45
3.1 Introduction 45
3.2. Materials 45
3.2.1 Poly (methyl methacrylate) (PMMA) 45
3.2.2 Thermoplastic Polyurethane (TPU) 47
3.2.3 Carbon Dioxide (CO2) 48
3.3 Production of Blends 48
3.4 Foaming Experiment 49
3.5 Characterization 50
3.5.1 Melt Flow Index (MFI) 50
3.5.2 PMMA Purification 51
3.5.3 Differential Scanning Calorimetry (DSC) 51
3.5.4 Nanostructure of PMMA-TPU Blend 51
3.5.5 Rheological Behavior 52
3.5.6 CO2 Solubility Measurement 52
3.5.7 Foam Density 53
3.5.8 SEM Image Characterization 53
3.5.9 Open-cell Content 55
Chapter 4 Controlling the Structure and Density of PMMA Bimodal Nanocellular Foam by Blending Different Molecular Weights 56
4.1 Introduction 56
4.2 Experimental 58
4.2.1 Materials 58
4.2.2 PMMA Purification 59
4.2.3 PMMA blend production 59
4.2.4 CO2 solubility measurement 60
4.2.5 Foaming experiment 60
4.2.6 Rheological behavior 60
4.2.7 Foam Characterization 60
4.2.8 Open-cell content 61
4.3 Result and Discussion 62
4.3.1 PMMA Characterization 62
4.3.2 Physical Properties and Miscibility of the Blends 62
4.3.3 CO2 solubility in PMMA blends 65
4.3.4 Influence of PMMA-H content on foaming behavior 66
4.3.5 Formation of bimodal foam 75
4.3.6 Bimodal foam structure characterization 79
4.3.7 Effect of PMMA-H content on cell size, cell density, and open-cell content 82
4.3.8 The effect of molecular weight and relaxation time on cell structure 84
4.4 Conclusion 90
Chapter 5 Fabrication and characterization of low-density nanocellular foam based on PMMA/TPU blends 92
5.1 Introduction 92
5.2 Experimental section 94
5.2.1 Materials 94
5.2.2 PMMA-TPU blend production 94
5.2.3 Foaming experiment 95
5.2.4 Nanostructure of PMMA-TPU blend 95
5.2.5 CO2 solubility 95
5.2.6 Density and cellular structure 96
5.2.7 Rheological behavior 96
5.2.8 Open-cell content 96
5.3 Result and Discussion 97
5.3.1 Rheological properties 97
5.3.2 Phase morphology of PMMA-TPU blend 99
5.3.3. Cellular structure of PMMA-TPU blend 103
5.3.3.1 The effects of TPU hardness on PMMA-TPU foam 103
4.3.3.2 The effects of foaming temperature 113
4.3.3.3 Effects of saturation pressure and temperature 117
4.3.3.4 Relative density and cell size mapping 120
4.3.3.5 Nucleation efficiency 122
5.4 Conclusion 123
Chapter 6 Summary and Future Work 125
6.1 Short Summary 125
6.2 Future Work 127
References 128
Appendix I 147
Appendix II: The effects of molecular weight and CO2 solubility on the structure of PMMA nanocellular foam 149
Abstract 149
Introduction 149
Materials and Experiment 150
Result and discussion 151
Conclusion 153
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