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Physical and Chemical Adhesion of Complex Structured Biomaterial Particles: Pollen Exine and Cellulose Nanocrystal

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Physical and Chemical Adhesion of Complex Structured Biomaterial Particles: Pollen Exine and Cellulose Nanocrystal PHYSICAL AND CHEMICAL ADHESION OF COMPLEX STRUCTURED BIOMATERIAL PARTICLES: POLLEN EXINE AND CELLULOSE NANOCRYSTAL A Dissertation Presented to The Academic Faculty by Zihao Qu In Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy in the School of Chemical and Biomolecular Engineering Georgia Institute of Technology December 2017 COPYRIGHT © 2017 BY ZIHAO QU PHYSICAL AND CHEMICAL ADHESION OF COMPLEX STRUCTURED BIOMATERIAL PARTICLES: POLLEN EXINE AND CELLULOSE NANOCRYSTAL Approved by: Dr. J. Carson Meredith, Advisor Dr. Peter J. Ludovice School of Chemical and School of Chemical and Biomolecular Engineering Biomolecular Engineering Georgia Institute of Technology Georgia Institute of Technology Dr. Sven H. Behrens Dr. Min Zhou School of Chemical and School of Mechanical Engineering Biomolecular Engineering Georgia Institute of Technology Georgia Institute of Technology Dr. Elsa Reichmanis School of Chemical and Biomolecular Engineering Georgia Institute of Technology Date Approved: [October 24th, 2017] This work is dedicated to my family. ACKNOWLEDGEMENTS I would like to thank my family for giving me the courage and support needed to pursue a Ph.D. degree, I would not be where I am today without your endless love. I would like to thank my mother and father for teaching me to always have a positive altitude, for allowing me to grow up with great freedom and choose my own path. Their encouragement and support have always been there whenever I need. I would like to thank my elder brother, Qu Yang. I feel so lucky to have a brother like you, who always give support and protection throughout my life. Finally, I would like to thank my grandmother, for unconditional love, teaching me to have a strong will, and watching over me from heaven. I would like to sincerely thank my advisor, Dr. Carson Meredith, for all his guidance, patience and inspiration throughout my journey as a graduate student at Georgia Tech. I feel fortunate to have had him as my advisor. He set a great example for me to learn, with his great personality, high work ethic and strong integrity. I am especially grateful to his support and concern when I had to go back home for my family. I would like to thank my committee members. Dr. Sven Behrens, Dr. Elsa Reichmanis, Dr. Peter J. Ludovice, and Dr. Min Zhou for their support and valuable feedback throughout my Ph.D. education. Special appreciation is given to Dr. Meisha Shofner, Dr. Greg Schueneman and Dr. Eric Mintz for their regular support and collaboration. Additionally, I would like to acknowledge the organizations that provided funding for my research: the U.S. Air Force Office for Scientific Research, and the U.S.D.A. Forest Products Laboratory iv I would like to thank all the past and current members of the Meredith research group, Dr. Haisheng Lin, Dr. Ismael Gomez, Dr. Jie Wu, Dr. Zifu Li, Dr. Oluwatimilehin Fadiran, Dr. Natalie Girouard, Dr. Yi Zhang, Dr. Donglee Shin, Songcheng Wang, Chinmay Satam, Scott Essenmacher, Ezgi M. Dogan Guner, for sharing their knowledge and support along with enjoyable moments. Last but not least, I would like to thank my girlfriend, Xi Yizhao, whose love and support have made this work possible. v TABLE OF CONTENTS ACKNOWLEDGEMENTS iv LIST OF TABLES ix LIST OF FIGURES x SUMMARY xv CHAPTER 1. INTRODUCTION 1 1.1 Background 1 1.2 Basic physical principles of adhesion 2 1.2.1 Dry adhesion based on van der Waals approach 2 1.2.2 Dry adhesion based on contact mechanics 7 1.2.3 Adhesion theories in composite materials 9 1.3 Pollen exine as a model particle with complex microstructured morphology 12 1.3.1 Pollen grains structure 12 1.3.2 Pollen exine chemistry 15 1.3.3 Mechanical property of pollen exine 16 1.3.4 Atomic force microscopy for adhesion measurements 18 1.4 Polymer composite and cellulose nanocrystal 19 1.4.1 Polymer composite overview 19 1.4.2 Cellulose nanocrystals as composite fillers 21 1.4.3 Acrylic polymer composite 24 1.5 Thesis overview 26 CHAPTER 2. INTERACTION OF COMPLEX MICROSTRUCTURED PARTICLES: ROLES OF ADHESION, GEOMETRY AND FRICTION 28 2.1 Overview 28 2.2 Introduction 29 2.3 Experimental methods 31 2.3.1 Materials 31 2.3.2 Pollen preparation 32 2.3.3 Colloidal probe and substrate preparation 33 2.3.4 Scanning electron microscopy (SEM) 33 2.3.5 Interaction force measurement 34 2.4 Results and discussions 36 2.4.1 Morphology of cleaned sunflower pollen 36 2.4.2 Adhesion forces between the same probe pollen and different substrate pollens in “Top” configuration 37 2.4.3 Adhesion forces between the same pair of pollens with different configurations 41 2.4.4 Force-distance curves of pollen-pollen interaction 42 2.4.5 Quantitative model for pollen-pollen interaction 45 vi 2.5 Conclusion 53 CHAPTER 3. MODULUS OF SPOROPOLLENIN DETERMINED BY DIRECT NANOINDENTATION MEASUREMENT OF POLLEN EXINE 54 3.1 Overview 54 3.2 Introduction 55 3.3 Experimental methods 59 3.3.1 Materials 59 3.3.2 Sample preparation 59 3.3.3 Scanning electron microscopy (SEM) 60 3.3.4 Peak Force Quantitative Mechanical Properties Mapping (PFQNM). 60 3.3.5 Probe selection 65 3.3.6 Probe calibration 65 3.4 Results and discussion 67 3.4.1 Pollen morphology 67 3.4.2 Probe calibration 68 3.4.3 Morphology effect 73 3.4.4 Probe effect 75 3.4.5 Effect of acid-base Treatment 77 3.4.6 Effect of water vapor exposure 78 3.4.7 Comparison with other biomaterials 80 3.5 Conclusion 81 CHAPTER 4. ACRYLIC FUNCTIONALIZATION OF CELLULOSE NANOCRYSTALS WITH 2-ISOCYANATOETHYL METHACRYLATE 83 4.1 Overview 83 4.2 Introduction 84 4.3 Experimental methods 86 4.3.1 Materials 86 4.3.2 Preparation of IEM-CNC 87 4.3.3 Attenuated total reflectance fourier transform infrared spectroscopy (ATR- FTIR). 87 4.3.4 X-ray photoelectron spectroscopy (XPS). 88 4.3.5 Solid state 13C NMR 88 4.3.6 Elemental analysis. 89 4.3.7 X-ray diffraction (XRD) 89 4.3.8 Thermogravimetric analysis (TGA) 89 4.3.9 Contact angle measurement 90 4.4 Results and discussion 90 4.4.1 Characterizing the chemistry of modified CNCs 90 4.4.2 Crystallinity of um-CNCs and m-CNCs 96 4.4.3 Thermal stability of um-CNCs and m-CNCs 97 4.4.4 Enhanced hydrophobicity of m-CNCs 98 4.5 Conclusion 99 vii CHAPTER 5. MECHANICAL PROPERTIES OF ACRYLIC FUNCTIONALIZED PMMA/CNC COMPOSITES: THE EFFECT OF SURFACE MODIFICATION OF CNC AND OPTIMIZED PREPARATION PROCESS 101 5.1 Overview 101 5.2 Introduction 102 5.3 Experimental methods 103 5.3.1 Materials 103 5.3.2 Eliminate toluene from m-CNCs/toluene organogel 103 5.3.3 Solution polymerization and solution casting method 104 5.3.4 Bulk polymerization and hot pressing 105 5.3.5 Solution polymerization and precipitation 106 5.3.6 ATR-FTIR 106 5.3.7 Gel permeation chromatography (GPC) 107 5.3.8 Differential scanning calorimetry (DSC) 107 5.3.9 TGA 107 5.3.10 Polarized light microscopy (PLM) 108 5.3.11 UV-vis spectroscopy 108 5.3.12 Tensile testing 108 5.3.13 Scanning electron microscopy (SEM) 109 5.4 Results and discussion 109 5.4.1 Solution-casting method 109 5.4.2 Bulk-pressing method 118 5.4.3 Solution-pressing method 124 5.5 Conclusion 132 CHAPTER 6. CONCLUSIONS AND RECOMMENDATIONS 134 6.1 Summary and Conclusions 134 6.1.1 Investigate micro particle-particle adhesion with a complex morphology 134 6.1.2 Investigate nano particle-matrix adhesion with tailored surface chemistry 136 6.2 Recommendation and future work 138 6.2.1 Investigate the effect of different morphology on particle-particle adhesion 138 6.2.2 Hybrid modification of CNCs 139 REFERENCES 141 viii LIST OF TABLES Table 2.1 Characteristics of sunflower pollen grains and surface morphology 37 from SEM image analysis Table 2.2 Characteristic behaviors of the force-distance curves of pollen-pollen 43 and pollen-silicon wafer interaction. Table 2.3 Dimensions of sunflower pollens used in the model. 49 Table 3.1 AFM probes used in this work. 65 Table 3.2 Dimensions of pollen grains 68 Table 3.3 Tip radii measured or estimated by different methods before and after 73 AFM measurement of pollens. Table 3.4 Young’s modulus of representative biomaterials. 81 Table 4.1 Elemental Composition of um-CNCs and m-CNCs 96 Table 4.2 The onset temperature of degradation. 98 Table 5.1 The molecular weight of PMMA composite with 0.5, 1.0, 2.0% m- 112 CNC, and 2.0% um-CNC. Table 5.2 Tg of neat PMMA and um-CNC composite, the heating range is from 118 20oC to 160oC Table 5.3 Tg of neat PMMA, um-CNC and m-CNC composite, the heating 118 range is from 20 oC to 200 oC ix LIST OF FIGURES Figure 1.1 Attractive van der Waals force F between two curved mica 4 surfaces of radius 푹 ≈ ퟏ 풄풎 measured in water and aqueous electrolyte solutions. It showed retardation effect beyond about 5 nm. This figure is taken from reference [23]. Figure 1.2 Van der Waals interaction energy and force between 5 macroscopic bodies of common geometries. This figure is taken from reference [23]. Figure 1.3 Regions of surface forces action according to (a) the JKR model, 9 (b) the DMT model, and (c) Maugis model. Figures are taken from reference [33].
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