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Synthesis and Characterization of In-Situ Nylon-6/Epoxy Blends

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Synthesis and Characterization of In-Situ Nylon-6/Epoxy Blends Synthesis and Characterization of in-situ Nylon-6/Epoxy Blends A thesis submitted to the Division of Research and Advanced Studies University of Cincinnati In partial fulfillment of the requirements for the degree of Master of Science 2016 In the Materials Science and Engineering Program, The Department of Mechanical and Materials Engineering By Anushree Deshpande B.E Polymer, University of Pune, 2011 Committee Members: Dr. Jude O. Iroh (Chair) Dr. Relva C. Buchanan Dr. Raj M. Manglik 1 ABSTRACT Epoxy is a thermosetting polymer known for its excellent adhesion, thermal stability, chemical resistance and mechanical properties. However, one of the major drawbacks of epoxies is its inherent brittleness. In order to overcome this drawback, incorporation of a thermoplastic as a second phase has proven to improve the impact strength without affecting the mechanical properties of epoxy. Researchers in the past have studied polyamide/epoxy blends in terms of blend compatibility, thermo-mechanical properties and morphology via solution blending. The current research effort employs in-situ polymerization to synthesize polyamide/epoxy blends. Blends of various compositions were synthesized by introducing Ɛ-Caprolactam (monomer of nylon-6) in the prepolymer of epoxy. All blend fractions were cured by exposing them to the same time and temperature conditions; and characterized using Dynamic Mechanical Analysis (DMA), Fourier Transform Infrared Spectroscopy (FTIR), Brookfield Viscometry, Scanning Electron Microscopy (SEM) and Thermogravimetric Analysis (TGA). DMA results show an overall increase in glass transition temperature and storage modulus in the rubbery region. FTIR results reveal maximum epoxy curing up to 15 wt% monomer loading, beyond which the plateauing of the epoxy conversion is recognized. Shear viscosity measurements, along with FTIR and DMA results reveal increased interactions between Ɛ-Caprolactam and epoxy. TGA results display improved thermal stability till 250oC after which the degradation onset of the in-situ nylon-6/epoxy blend shifts to lower temperatures with respect to the neat nylon-6 and neat 2 epoxy. SEM micrographs reveal absence of Nylon-6 agglomerates in the blend indicating improved dispersion of nylon-6 in epoxy. Moreover, this study draws a comparison between in-situ and ex-situ blending of polyamide and epoxy, with respect to trends obtained in glass transition temperature (Tg), storage modulus and nature of dispersion. Nylon-6/epoxy blends processed via ex-situ blending possessed reduced storage modulus and glass transition temperature with good damping properties compared to neat epoxy. On the other hand, reactive blends of nylon-6/epoxy processed via in-situ polymerization of Ɛ- Caprolactam in presence of epoxy prepolymer resulted in a material with increased modulus and high glass transition temperature and improved dispersion of filler phase in the matrix phase due to reduced agglomeration of nylon-6. 3 4 ACKNOWLEDGEMENTS First, I would like to thank my research advisor, Dr. Jude Iroh for his insightful comments and guidance all through my research and for allowing me the freedom to explore different ideas. I appreciate his patience and steadfast support which helped me overcome difficult times. I would like to thank Dr. Relva Buchanan and Dr. Raj Manglik for serving on my defense committee. I would like to thank Dr. Aniket Vyas for training me on the synthesis and lab instruments, and providing useful inputs based on his experience in ex-situ blending during the course of my research. Moreover, I am extremely thankful to my lab members- Shirley Peng, Dr. Patricia Okafor, Praveen Balasubramani, Nathan Holliday, Yujie Zhang, Xueying He, Wajeeh Marashdeh, Jehan Kothari, Caroline, Brent Huxel for their help and support and for making this journey through graduate school an enjoyable one. I dedicate this work to my parents who have been a constant source of emotional strength and support and I thank them for encouraging me to pursue my dreams to study at the University of Cincinnati. Lastly, I would like to thank Dr. Necati Kaval for allowing timely access to the Spectroscopy Lab and training me on Fourier Transform Infrared Spectroscopy instrument. 5 TABLE OF CONTENTS Abstract 2 Acknowledgements 5 List of Tables 8 List of Figures 10 Chapter 1: Introduction………………………………………………………………………….15 1.1. Synthesis routes for Polymer blends…………………………………………….….15 1.2. Incorporation of thermoplastic in Epoxy……………………………….………….16 1.3. Incorporation of Nylon in Epoxy……………………………………………………17 1.4. Significance of in-situ blending……………………………………………………...18 1.5. Epoxy Resin……………………………………………………………………..…....19 1.5.1. Types of Epoxy Resins………………………………………………...…...20 1.5.1a. Bisphenol A type resins…………………..……………….……...20 1.5.1b. Bisphenol F type resins…………………………………………...21 1.5.1c. Multifunctional epoxy resin……………………………..……….21 1.5.1d. Novolac Epoxy Resin………………………………………..……22 1.5.1e. Cycloaliphatic Epoxy resin…………………………………..…...23 1.6. Curing of Epoxy………………………………………………...................................23 1.7. Nylon-6………………………………………………..................................................25 1.8. Synthesis Routes of Polyamide-6…………………………………………….……...25 1.9 Research Objective…………………………………………………………………...26 Chapter 2: Experimental………………………………………………………………….……...28 2.1. Materials……………………………………………………………………………...28 2.2. Synthesis of neat Nylon-6……………………………………………………………28 6 2.3. In-situ synthesis of Nylon-6/Epoxy reactive blends…………………………..……28 2.4. Sample preparation for neat Epoxy (control)……………………………….……..30 2.5. Cure Conditions………………………………………………………………...……30 2.6. Characterization Techniques…………………………………………………….….31 2.6.1. Fourier Transform and Infrared Spectroscopy - Attenuated Total Reflectance (FTIR-ATR)…………………………………………….………….. 31 2.6.2. Dynamic Mechanical Analysis (DMA)…………………………………....31 2.6.3. Scanning Electron Microscopy (SEM)………………..…………….…….32 2.6.4. Thermogravimetric Analysis (TGA)………………………………….…..33 2.6.5 Shear Viscometry…………………………………………………….……..33 Chapter 3: Results & Discussion………………………………………………………………...36 3.1. Reactive blends of Nylon-6 & epoxy……………………………………………..36 3.1.1 Fourier Transform Infrared (FTIR) Spectroscopy Analysis…………..36 3.1.1a. FTIR analysis of Ɛ-caprolactam…………………………………………36 3.1.1b. FTIR analysis of neat Epoxy……………………………………………..37 3.1.1c. FTIR analysis of Ɛ-caprolactam in Epoxy during in-situ synthesis……38 3.1.1d. FTIR Analysis of Nylon-6/Epoxy blends compositions after curing…..38 3.1.1e. FTIR Analysis of neat Nylon-6 synthesized at 80oC……………………39 3.1.1f. FTIR Analysis of Epoxy conversion……………………………………..40 3.2. Dynamic Mechanical Analysis (DMA) …………………………………………..41 3.2.1. Analysis of Tan delta peaks……………………………………………..…42 3.2.2. Analysis of Storage moduli…………………………………………..…….45 3.3. Shear Viscometry…………………………………………………………………47 3.3.1. Effect of Nylon-6 monomer loading on shear viscosity………………….48 7 3.3.2. Effect of change in temperature on shear viscosity……………………...48 3.3.3. Effect of increase in polymerization time on shear viscosity……………50 3.4. Thermogravimetric Analysis (TGA)……………………………………….……….51 3.5. Comparison between ex-situ and in-situ method of blending………..……………53 Chapter 4: Conclusion………………………………………………………………………...56 Chapter 5: Future Work and Suggestions……………………………………………..…….58 References………………………………………………………………………………..………..59 Figures………………………………………………………………………………………..…....65 Appendix……………………………………………………………………………………..…..105 8 LIST OF TABLES Table 1: Compositions for in-situ Nylon-6/Epoxy blends Table 2: Cure conditions Table 3: Absorbance peaks for Ɛ-caprolactam Table 4: Absorbance peaks for neat Epoxy Table 5: Absorbance peaks for Nylon-6 Table 6: Summary of Tan delta peak analysis Table 7: Summary of Storage moduli analysis Table 8: Summary of Activation energies for 2.5wt% and 30wt% NY-EP blends Table 9: Degradation temperatures for Nylon-6 and Epoxy in the in-situ blends 9 LIST OF FIGURES Figure 1: Structure of an Oxirane Ring Figure 2: Structure of Bisphenol A oligomer Figure 3: Structure of Bisphenol F oligomer Figure 4: Triglycidyl derivative of p-amino phenol Figure 5: Tetraglycidylmethylene dianiline (TGDDM) Figure 6: Epoxy Novolac Resin Figure 7: Cycloaliphatic Epoxy Figure 8: Epoxy Curing mechanism by an amine Figure 9: Structure of Nylon-6 Figure 10: Schematic representation of Nylon-6 synthesis Figure 11: Schematic of a typical DMA graph Figure 12: Schematic of a TGA thermogram Figure 13: Structure of Ɛ-Caprolactam (monomer of Nylon-6) Figure 14: FTIR spectrum of Ɛ-caprolactam (monomer) showing presence of N-H stretch, hydrocarbon stretch, carbonyl (C=O) of the amide Figure 15: Structure of an Epoxy resin molecule Figure 16: FTIR spectrum of neat epoxy showing the presence of hydroxyl (O-H) at 3402 cm-1, (C-H) at 2927 cm-1, (C-C) of the benzene ring and oxirane ring at 914cm-1 Figure 17: FTIR spectrum at the start of synthesis where caprolactam was dispersed in neat epoxy at room temperature of 25oC Figure 18. FTIR spectrum during blend synthesis of caprolactam in neat epoxy at 65oC. Figure 19: FTIR spectrum of thermally cured 5 wt% in-situ nylon-6/epoxy blend showing the absence of (C=O) carbonyl bond of the amide group Figure 20. FTIR spectrum of thermally cured 10 wt% in-situ nylon-6/epoxy blend showing a slight shoulder at 1649 cm-1 attributed to the (C=O) carbonyl bond of the amide group 10 Figure.21 FTIR Spectrum of thermally cured 15 wt% in-situ nylon-6/epoxy blend showing increased absorption of the amide carbonyl (C=O) at 1643cm-1 Figure 22. FTIR spectrum of thermally cured
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