使用 CO2 和 N2 發泡劑生產和表徵 TPU 泡｜國立臺灣科技大學博碩士論文系統

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研究生：	RAGHAVENDRAKUMAR RANGAPPA RAGHAVENDRAKUMAR RANGAPPA
論文名稱：	使用 CO2 和 N2 發泡劑生產和表徵 TPU 泡 Production and Characterization of TPU Foam by Using CO2 and N2 Blowing agents
指導教授：	葉樹開 Shu-Kai Yeh
口試委員:	葉樹開 Shu-Kai Yeh 邱方遒 Fang-Chyou Chiu 童世煌 Shih-Huang Tung 賴森茂 Sen Mao Lai 何明樺 Ming-Hua Ho
學位類別：	博士 Doctor
系所名稱：	工程學院 - 材料科學與工程系 Department of Materials Science and Engineering
論文出版年：	2023
畢業學年度：	111
語文別：	英文
論文頁數：	231
中文關鍵詞：	熱塑性聚氨酯泡材、硬度、成核劑、發泡劑、二氧化碳、氮氣、混煉、塑化
外文關鍵詞：	Thermoplastic polyurethane foam, hardness; nucleating agents;, blowing agents; CO2; N2;, extrusion;, plasticization
相關次數：	點閱：318 下載：0
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熱塑性聚氨酯 (TPU) 泡材是緩衝、運動鞋、航太、運輸、生物醫學、電磁屏蔽、傳感、智能響應、建築、電子和包裝應用的理想輕質材料. 最近，新興起的發泡熱塑性聚氨酯 (ETPU) 製成的泡材，由於具有可回收性，逐漸取代傳統的交聯乙基醋酸乙烯酯 (EVA) 泡材已被取代。
發泡TPU不同於硬質發泡高分子，因為TPU存在發泡後收縮的問題，很難製備低密度的TPU泡材。在本論文中，我們使用PTMEG-MDI/BD 基 TPU 做為基材，並使用 CO2 和 N2 等物理發泡劑製備為發泡材料。我們研究了混煉、成核劑、發泡劑和硬度對 TPU 發泡行為和物理性能的影響。我們的研究成功製備了具有超過 6 倍膨脹、具有緻密泡孔結構和有限收縮的 TPU 泡材。由於 TPU 的低模量和 CO2 的高擴散率，目前仍然很難使用 CO2 作為發泡劑製備彈性體泡材。
然而，使用氮氣作為發泡劑可以克服這些缺點。N2 高壓釜發泡技術是製備 TPU 泡材的環保技術。製備的泡材具有優異的尺寸穩定性，收縮率小於 4%。因此，N2 是解決 TPU 泡材收縮的優良發泡劑。此外，使用氮氣製備的泡材泡孔尺寸更小、泡孔密度更高。本論文還報告了一個獨特的現象。將 N2 溶解在 TPU 中不僅會降低熔點，也會降低結晶度。在高壓N2下退火對具有高軟段含量的 TPU 顯示出顯著的塑化效果。不完全有序晶體的熔融峰在 100°C 左右完全消失。該研究有助於了解N2塑化對TPU結晶的影響以及氮氣發泡技術的發展。

Thermoplastic polyurethane (TPU) foam is an ideal lightweight material for cushioning, sports shoes, aerospace, transportation, biomedical, electromagnetic shielding, sensing, intelligent response, construction, electronics, and packaging applications. Recently, thermoplastic polyurethane (TPU) foam gradually replaced crosslink ethyl vinyl acetate (EVA) foams due to their recyclability.
Foaming TPU differs from foaming rigid plastics because TPU has post-foam shrinkage problems, which makes it difficult to fabricate low-density TPU foams. It is still challenging to fabricate elastomeric foams with limited shrinkage and good surface quality using CO2 as a blowing agent because the low modulus of TPU and high diffusivity of CO2 led to foam shrinkage. This study used PTMEG-MDI/BD-based TPU as a polymer matrix. The microcellular foams were produced using physical blowing agents (PBAs) such as CO2 and N2. The effect of extrusion, nucleating agents, blowing agents, and hardness on the foaming behavior and physical properties of TPU were studied.
Extrusion significantly influences the thermal and mechanical properties and foaming behavior of TPUs. Although the molecular weight decreased significantly after extrusion, the re-distribution of hard segments in the TPU caused the cell density to increase by 30 to 50 times. In addition, the elongation at the break of the TPU solids increased by 40%. The cell size, expansion ratio, cell density, shrinkage versus saturation temperature (Tsat), and saturation pressure (Psat) were also studied extensively. The results show that Tsat significantly affects the expansion ratio, and Psat has more impact on foam shrinkage, while extrusion processing has little impact on foam shrinkage.
On the other hand, the effect of N2 dissolution on the thermal behavior of polyether-based thermoplastic polyurethanes (TPUs) was extensively investigated. Dissolving N2 in TPU reduced the melting point but decreased crystallinity. A weight-loss-based test showed that the N2 sorption increased with increased soft segment (SS) content. Annealing with N2 showed an apparent plasticizing effect on TPU with high SS content. The melting peak of imperfectly ordered crystals, around 100°C, completely disappeared. This research contributes to understanding the impact of N2 plasticization on TPU crystallization and the development of nitrogen foaming technology. Using N2 as a PBA is an eco-friendly foaming method to overcome foam shrinkage problems. At the maximum expansion ratio, the N2-blown foams exhibited a fine cell structure with a shrinkage ratio of less than 4%. As a result, N2 might be an excellent blowing agent for TPU to solve the foam shrinkage problem.

Contents                                                                                                                           Pages
摘要    i
Abstract    ii
Acknowledgments    iv
List of Contents    vi
List of Figures    xi
List of Tables    xv
List of Abbreviations and Symbols    xvi
Chapter 1 Introduction    1
1 Background of the study    1
2 Elastomeric foam    4
2.1 Thermoplastic polyurethanes foam    6
3 Physical foaming of thermoplastic foam    7
4 Research Motivation    8
5 Objective of the thesis    9
6 Thesis structure    9
Chapter 2 Literature Review    12
1 The Fundamentals of Polymer Foaming    12
2 Type of polymer foam    12
3 Foaming technologies    14
3.1 Blowing agents    17
4 Cell Nucleation    20
4.1 Homogenous nucleation    22
4.2 Heterogeneous Nucleation    24
4.3 Nucleating agents induced heterogeneous nucleation    28
4.4 Crystals-induced heterogeneous nucleation    31
4.5 Gas-induced polymer crystallization/plasticization    32
5 Foam shrinkage    35
6 Classification of the thermoplastic elastomers foaming process    39
6.1 Batch foaming    39
6.2 Autoclave bead foaming and molding    41
6.3. Continuous extrusion foaming    43
6.4 Molding of bead foams    45
6.5 Foam injection molding    50
6.6 Compression foam molding    52
7 General Properties and Applications of thermoplastic elastomers foam    53
7.1 Relative density    54
7.2 Mechanical properties    54
7.3 Thermal properties    56
7.4 Energy Absorption Properties    58
7.5 Acoustical Properties    59
7.6 General Applications of TPE foam    60
8 Summary    60
Chapter 3 Materials and Experimental Methods    63
1 Introduction    63
2 Materials    63
2.1 Chemistry of Thermoplastic Polyurethane    63
2.2 Talc and Silica Used as Nucleating Agents    66
2.3 Carbon dioxide and Nitrogen used as Blowing agents    68
3 Sample preparation    70
3.1 Dog-bone shape TPU sample    70
3.2 Circular Shape TPU sample    70
4 One-step Batch Foaming Experiment    71
5 Characterization    72
5.1 Isothermal annealing analysis    72
5.2 Differential Scanning Calorimeter (DSC)    72
5.3 Thermogravimetric analysis (TGA)    73
5.4 Thermomechanical Analysis (TMA)    73
5.5 Mechanical properties measurement    74
5.6 Rheology experiment    75
5.7 Hardness measurement    76
5.8 N2 sorption behavior    76
5.9 Foam density expansion and shrinkage ratio measurement    76
5.10 Cell Analysis    77
Chapter 4     Effect of Extrusion, Nucleating Agents, and Processing Parameters on the Foaming Behavior of Thermoplastic Polyurethane with Different Hard Segments    79
1 Introduction    79
2 Experimental methods    81
2.1 Materials    81
2.2 Sample Preparation    82
2.3 Material characterization    82
2.4 Thermal analysis    82
2.5 Batch foaming    82
2.6 Foam Structural characterization    83
3 Results and discussion    83
3.1 Effect of extrusion on physical properties of TPU at different hardness levels    83
3.2 Mechanical properties    84
3.3 Softening point    86
3.4 Differential Scanning Calorimeter (DSC) Thermal Analysis    86
3.5 Effect of extrusion and foaming temperature on the foaming behavior    90
3.6 Effect of Psat on foaming behavior of TPU    94
3.7 Effect of nucleating agents on the foaming behavior    96
3.8 Effect of extrusion on shrinkage behaviour of foams    100
3.9 Effect of Tsat and Psat on the shrinkage behaviour foam    102
3.10 Effect of nucleating agents on the shrinkage of TPU foam    105
4. Conclusion    106
Chapter 5     Effect of N2 plasticization on the crystallization of different hardnesses of thermoplastic polyurethanes    108
1 Introduction:    108
2 Experimental methods    111
2.1 Materials    111
2.2 Melt compounding    111
2.3 Isothermal annealing analysis    111
2.4 Differential scanning calorimetry analysis    111
2.5 N2 sorption behavior    112
3 Results and discussion    113
3.1 Effect of post-annealing on the crystalline melting characteristics of TPUs    113
3.2 N2 Sorption in TPUs    120
3.3 Effect of annealing on the crystallization behavior of TPUs in the presence of N2    122
3.4 Effect of N2 pressure on the crystallization of TPU    127
4. Conclusion    129
5 Supplementary Material    131
5.1 TGA Analysis of TPU    131
5.2 Effect of thermal annealing on the crystallization behavior of TPUs    131
5.3 Effect of annealing on the crystallization behavior of TPUs in the presence of N2    132
5.4 ΔHm1 and ΔHm2 versus Ta    133
Chapter 6     Investigating the Role and Impact of N2 as a Blowing Agent in the Fabrication of Thermoplastic Polyurethane Foams    136
1 Introduction    136
2 Experimental methods    139
2.1 Materials    139
2.2 Melt compounding    139
2.3 Foaming process    139
2.4 Foam Structural characterization    140
3 Results and discussion    140
3.1 Effect of TPU hardness and temperature on the foaming behavior    140
3.2 Effect of pressure on foaming behavior of TPU foams    148
3.3 Dimensional stability of TPU foam    151
4 Conclusion    153
5 Supplementary material    155
Chapter 7 Summary and Future Work Recommendation    159
1 Summary    159
1.1 Effect of extrusion on the physical properties and foaming behavior of various hardness of TPU.    159
1.2 Effect of N2 plasticization on the crystallization behavior of TPU    160
1.3 Investigating the Role and Impact of N2 as a Blowing Agent in the Fabrication of Thermoplastic Polyurethane Foams    160
2 Future work recommendation    161
3 List of Publications and conferences    162
3.1 SCI Indexed Jounral Publications    162
3.2 Conferences Presentation with Proceeding:    163
References    164
Appendix I: Effect of Nanostructured Talc and Silica on Thermal, Rheological and foaming behavior of TPU Nanocomposites    195
AI-1 Talc and Silica dispersion in TPUs    195
Talc    195
Silica OX50    197
AI-2 Thermal Properties 85AU and 90AL with talc and OX50    198
AI-3 Effect of nucleating agents on the rheological behavior of TPU    201
AI-4 Effect of Talc and OX50 on the foaming behavior of 85AU and 90AL    204


                                

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全文公開日期 2028/05/17 (校內網路)
全文公開日期 2028/05/17 (校外網路)
全文公開日期 2028/05/17 (國家圖書館：臺灣博碩士論文系統)

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