微差掃描卡儀(DSC)與模數微差掃描卡儀(MDSC)被用來研究聚二醚酮(PEEK)之結晶動力學和熔融行為。DSC研究等溫結晶在290和320ºC之間，並且以Avrami分析法得到Avrami exponents和level-off time。這n1值變化從1.50到2.98而n2值是在0.52和1.37之間。發生雙熔融峰所需最小時間是藉由增加一分鐘間隔之等溫時間獲得，這個最小時間總是比level-off time長；因此level-off time不能表示單一或雙熔融峰行為的界限。為了瞭解雙熔融峰之熔融行為與機制，試片在400ºC下熔融15分鐘，然後等溫結晶在200和320ºC之間10或60分鐘且個別以10或2ºC/min加熱到380ºC。從結晶溫度在290和310ºC間之MDSC結果，發現兩個不同型態和熔融再結晶之現象共存。當等溫結晶溫度增加從290到310ºC，熔融再結晶對高熔融峰的貢獻將逐漸變小。而結晶溫度在320ºC時，雙熔融峰是由兩個不同型態之機制所導致。
以修正後之隔膜成形機製造[0/±45/90]2s均向複合材料。三種不同加工條件被用來製作相同結晶度但不同穿晶度的AS4/PEEK複合材料，長項張力-張力測試前後之型態藉由掃瞄式電子顯微鏡來觀察。穿晶度對短項張力測試沒有重要影響，這是由於[0/±45/90]2s疊層的0º板纖維主導在短項張力測試的高應力破斷。但當穿晶度增加，則長項張力測試破壞週數變長。這指示在[0/±45/90]2s的90º和45º板破壞起始之延遲而導致較長破壞週

Crystallization kinetics and melting behavior of PEEK were studied by differential scanning calriometry (DSC) and modulated differential scanning calriometry (MDSC). The isothermal crystallization was performed in DSC between 290 and 320°C. The Avrami constants (n1, n2) and the level off time were determined from the Avrami analysis. The n1 values varied from 1.50 to 2.98, and the n2 values were between 0.52 and 1.37. The minimum induction time required for the occurrence of double melting peaks was obtained by increasing the isothermal crystallization time in a interval per minute. It was found that the minimum time was always longer than the level off time, which cannot be used as the delimitation for the occurrence of single or double melting peaks. To study the melting behavior and the mechanisms of double melting peaks, the samples after melting at 400°C for 15 min were crystallized isothermally between 200 and 320°C for 10 or 60 min, and then they were heated to 380°C at 10 or 2 °C/min, respectively. From the MDSC results of crystallization temperatures between 280 and 310°C, it is found that two different morphologies and melting-recrystallization phenomenon coexisted. As the isothermal crystallization temperature increased from 280 to 310°C, the contribution of melting-recrystallization to the upper melting peak gradually decreased. In the case of 320°C, the mechanisms of double melting peaks were dominated by two different morphologies only.
Quasi-isotropic composites in the stacking sequence of [0/±45/90]2s were fabricated by a modified diaphragm forming apparatus. Three different processing conditions were used to prepare AS4/PEEK composites with the same crystallinity but different transcrystallinity. The morphology before and after the long-term tensile-tensile tests was observed by means of scanning electron microscope. The transcrystallinity has no significant effect on the short-term tensile test. This was due to the fibers in the 0° plies of [0/±45/90]2S laminates dominated the failure at high stress for the short-term tensile test. However, as the transcrystallinity increased, the failure cycles for the long-term tensile test became longer. This expressed that the delay of damage initiation in the 90° and ±45° plies of [0/±45/90]2s led to a longer failure cycles in the long-term tensile tests.

Table of Contents

Part Ⅰ Crystallization Kinetics and Melting Behavior of PEEK

List of Tables Ⅱ

List of Figures Ⅱ

Abstract Ⅶ

Chinese Abstract Ⅸ

Chapter 1. Introduction 1

Chapter 2. Experimental 6
2.1 Materials 6
2.2 Instruments 6
2.3 Samples Preparation 6
2.4 Differential Scanning Calorimetry (DSC) 7
2.5 Modulated Differential Scanning Calorimetry (MDSC) 7
2.6 Avrami Analysis 9
2.7 Experimental Flow Chart 10

Chapter 3. Results 13
3.1 Isothermal Crystallization Kinetics 13
3.2 Melting Behavior Studied by Conventional DSC 15
3.3 Melting Behavior Studied by Modulated DSC (MDSC) 16
3.4 Different Heating Rates 18

Chapter 4. Discussion 31

Chapter 5. Conclusion 39

Chapter 6. References 40
List of Tables

Table 1-1. Literature review of double melting peaks and the corresponding thermal history for different grades of PEEK. 4

Table 3-1. Analysis of isothermal crystallization kinetics of PEEK. 19

Table 3-2. The melting temperatures of total and reversible MDSC thermograms (and the absolute crystallinity) for PEEK specimens after melting at 400ºC for 15 min and then crystallizing isothermally at various temperatures for 60 min. 20


List of Figures

Figure 1-1. Chemical structure of PEEK. 1

Figure 2-1. A sinusoidal temperature oscillation is overlaid on the conventional linear temperature ramp 11

Figure 2-2. Experimental Flow Chart 12

Figure 3-1. Heat flow versus time for PEEK specimens after melting at 400ºC for 15 min and then crystallizing isothermally at 300, 310 and 320ºC, respectively. 21

Figure 3-2. Plot of log[-ln(1-Xc(t))] vs. log t for PEEK crystallized isothermally at 300ºC. 22

Figure 3-3. DSC thermograms at a heating rate of 10ºC/min for PEEK specimens after melting at 400ºC for 15 min and then crystallizing isothermally at (a) 290, (b) 300, (c) 310, and (d) 320ºC for various time. 23



Figure 3-4. DSC thermograms at a heating rate of 10ºC/min for PEEK specimens after melting at 400ºC for 15 min and then crystallizing isothermally at (a) 200~270ºC, and (b) 280~320ºC, for 10 min. 25

Figure 3-5. DSC thermograms at a heating rate of 2ºC/min for PEEK specimens after melting at 400ºC for 15 min and then crystallizing isothermally at (a) 200~270ºC, and (b) 290~320ºC for 60 min. 26

Figure 3-6. Variation of the melting temperature with the crystallization temperature at a heating rate of 10 or 2 ºC/min for PEEK specimens after melting at 400ºC for 15 min and then crystallizing isothermally for 10 or 60 min, respectively. 27

Figure 3-7. Modulated DSC thermograms at a heating rate of 2 ºC/min for PEEK specimens after melting at 400ºC for 15 min and then crystallizing isothermally at (a) 200 and 280ºC, (b) 290 and 300ºC, and (c) 310 and 320ºC, respectively, for 60 min.28

Figure 3-8. Three DSC heating thermograms for PEEK specimens after melting at 400ºC for 15 min and then crystallizing isothermally at 300ºC for 30 min. 30

Part Ⅱ Influence of Transcrystallinity on the Long-Term
Tensile-Tensile Property of AS4/PEEK Composites

List of Scheme Ⅴ

List of Tables Ⅴ

List of Figures Ⅴ

Abstract Ⅶ

Chinese Abstract Ⅸ

Chapter 7. Introduction 45

Chapter 8. Experimental 51
8.1 Materials 51
8.2 Instruments 51
8.3 Specimens Preparation 51
8.4 Short- and Long-Term Tests 53
8.5 Scanning Electron Microscope (SEM) 53
8.6 Crystallinity Measurement 54
8.7 Experimental Flow Chart 54

Chapter 9. Results and Discussion 59
9.1 Processing-Morphology Relationships 59
9.2 Morphology-Mechanical Properties Relationships 62
9.2.1 Short-Term Tensile Test 62
9.2.2 Long-Term Tensile Test 63
9.3 Fractography and Failure Mechanisms 63

Chapter 10. Conclusion 76

Chapter 11. References 77

List of Scheme

Scheme 8-1 Three process conditions of [0/±45/90]2S AS4/PEEK composites. 55


List of Tables

Table 9-1. Crystallinity and tensile properties of [0/±45/90]2S AS4/PEEK composites. 66


List of Figures

Figure 7-1. Melting temperature is at 415ºC for 15 min, and the cooling rate is 10ºC/min. (a) 300ºC and (b) room temperature. 49

Figure 7-2. Schematic representation of a fiber reinforced semicrystalline thermoplastic system. 50

Figure 8-1. Schematic of modified diaphragm forming apparatus. 56

Figure 8-2. Geometry and dimension of the test specimen (in mm). 57

Figure 8-3. Schematic plot of flow chart. 58

Figure 9-1. DSC melting traces of [0/±45/90]2S AS4/PEEK composites with different process conditions. The heating rate was 20°C/min. 67

Figure 9-2. SEM micrographs of specimens after plasma etching. (a) HF; (b) LF. 68

Figure 9-3. SEM micrograph of HS specimen after plasma etching. 69

Figure 9-4. The excess free energy of solid clusters for homogeneous and heterogeneous nucleation. 70



Figure 9-5. (a) Variation of ∆G* with undercooling (∆T) for homogeneous and heterogeneous nucleation. (b) The corresponding nucleation rates assuming the same critical value of ∆G*. 71

Figure 9-6. Influence of process conditions on the failure cycles of [0/±45/90]2S AS4/PEEK composites under tensile-tensile loading at three applied stresses. 72

Figure 9-7. SEM micrographs of 90° plies fracture surface for [0/±45/90]2S AS4/PEEK composites processed under: (a) HF; (c) LF; (e) HS conditions. (b) (d) (f): A close-up of the arrow in (a) (c) and (e), respectively 73

Figure 9-8. SEM micrographs of 45° plies fracture surface for [0/±45/90]2S AS4/PEEK composites processed under: (a) HF; (c) LF; (e) HS conditions. (b) (d) (f): A close-up of the arrow in (a) (c) and (e), respectively. 74

Figure 9-9. SEM micrographs of 0° plies fracture surface for [0/±45/90]2S AS4/PEEK
composites processed under: (a) HF; (c) LF; (e) HS conditions. (b) (d) (f): A close-up
of the arrow in (a) (c) and (e), respectively. 75

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