Micro- and Nanostructured Epoxy/Rubber Blends
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1. Edition September 2014
464 Pages, Hardcover
170 Pictures (20 Colored Figures)
Monograph
Short Description
From the liquid stage, via phase separation, up to the final network, this book covers all aspects of epoxy toughening, resulting in a comprehensive review of the latest R&D in the field, explaining in detail thermal, optical, mechanical and electrical characterization methods
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Epoxy resins are polymers which are extensively used as coating materials due to their outstanding mechanical properties and good handling characteristics. A disadvantage results from their high cross-link density: they are brittle and have very low resistance to crack growth and propagation. This necessitates the toughening of the epoxy matrix without impairing its good thermomechanical properties. The nal properties of the polymer depend on their structure. The book focuses on the microstructural aspects in the modi cation of epoxy resins with low molecular weight liquid rubbers, one of the prime toughening agents commonly employed.
The book follows thoroughly the reactions of elastomer-modi ed epoxy resins from their liquid stage to the network formation. It gives an in-depth view into the cure reaction, phase separation and the simultaneous development of the morphology. Chapters on ageing, failure analysis and life cycle analysis round out the book.
INTRODUCTION
Epoxy Resin - Introduction
Cure Reactions
Curing Agents
Catalytic Cure
Co-reactive Cure
Primary and Secondary Amines
Mercaptans
Isocyanates
Carboxylic Acids
Acid Anhydrides
Different Curing Methods
Thermal Curing
Microwave Curing
Radiation Curing
Electron Beam Curing
Gamma Ray Irradiation
Curing of Epoxy Resins: Structure-Property Relationship
Toughening of Epoxy Resin
Different Toughening Agents
Liquid Elastomers for Toughening Epoxy Matrices
Rigid Crystalline Polymers
Hygrothermal Toughening Agents
Core-Shell Particles
Nanoparticles for Epoxy Toughening
Thermoplastic Modification of Epoxy Resin
Block Copolymers as Modifiers for Epoxy Resin
Rubber-Modified Epoxy Resin: Factors Influencing Toughening
Concentration Effects
Particle Size and Distribution of Rubber
Effect of Temperature
Effect of Rubber
Interfacial Adhesion
Toughening Mechanisms in Elastomer-Modified Epoxy Resins
Particle Deformation
Shear Yielding
Crazing
Simultaneous Shear Yielding and Crazing
Crack Pinning
Cavitation and Rumples
Quantitative Assessment of Toughening Mechanisms
Introduction of Chapters
LIQUID RUBBERES AS TEOUGHENING AGENTS
Introduction
Toughening of Thermoset Resins
Fracture Behavior of Rubber-Toughened Thermosets
Natural Rubbers
Preparation Method of LNR
Oxidation in the Presence of Redox System
Oxidation by Photochemical Method
Oxidation at High Temperatures and High Pressures
Oxidation by Cleavage Reagent Specific to Double Bonds
Metathesis Degradation
Liquid-Toughening Rubber in Thermoset Resins
Concluding Remarks
NANOSTRUCTURED EPOXY COMPOSITES
Introduction
Preparation Methods of the Nanostructured Epoxy Thermoset
Morphology of the Nanostructured Epoxy Thermoset
Parameters Controlling the Morphologies
Blends Composition
The Choice of Curing Agent
Topological Architecture of the Copolymer
Microphase Separation Mechanism
Self-Assembly Mechanism
Reaction-Induced Microphase Separation Mechanism
Mechanical and Thermal Properties
Fracture Toughness
Glass Transition Temperature
Conclusions and Outlooks
MANUFACTURE OF EPOXY RESIN/LIQUID RUBBER BLENDS
Introduction
Comparison of Hardeners
Rubber-Toughened Epoxy Resins
Cure Reaction Analysis
Conclusions
CURUE AND CURE KINETICS OF EPOXY-RUBBER SYSTEMS
Introduction
Cure Analysis
Curing Kinetics
Kinetics Analysis
Autocatalytic Model
Activation Energies
Dynamic Kinetics Methods
Isothermal Methods
Diffusion Factor
Differential Scanning Calorimetry
Dynamic DSC
Isothermal DSC
FTIR Spectroscopy
Dielectric Spectroscopy Thermal Method
Pressure-Volume-Temperature (PVT) Method
Dynamic Mechanical Analysis (DMA) and Rheological Methods
Conclusions
Acknowledgments
THEORETICAL MODELING OF THE CURING PROCESS
Introduction
Modeling of the Curing Kinetics
Mechanistic Approach
Phenomenological Models Describing the Reaction
nth-Order Model
Autocatalytic Model
Kamal and Sourour Model
Bailleul Model
Rheological Models
Gel Time Model
Viscosity Model
Effect of Vitrification (Tg ) on the Reaction Rate
Applications of the Empirical Models
Conclusion
PHASE-SPARATION MECHANISM IN EPOXY RESIN/RUBBER BLENDS
Introduction
Thermodynamics of Phase Separation
Nucleation and Growth Mechanism
Spinodal Decomposition
Phase Separation in Uncured Epoxy Resin/Liquid Rubber Blends
Phase-Separation Mechanism in Cured Blends
Conclusion
MORPHOLOGY ANALYSIS BY MICROSOPY TECHNIQUES AND LIGHT SCATTERING
Introduction
Developments of Morphology Analysis in Rubber-Modified Epoxies
Optical Microscopy (OM)
Scanning Electron Microscopy (SEM)
Atomic Force Microscopy (AFM)
Transmission Electron Microscopy (TEM)
Small-Angle Light Scattering (SALS)
Different Types of Morphologies
Phase-Separation Morphology of Epoxy/Rubbers Blends
Morphology of Hybrids
Homogeneous Morphology
Morphology of Toughening and Reinforcing Effects
Conventional Additives
Hyperbranched Polymers
Conclusions
Acknowledgments
PRESSURE-VOLUME-TEMPARATURE (PVT) ANALYSIS
Introduction
Generalities on the Behavior of the Polymers
Measurement Techniques
PvT Measures on Epoxies
RHEOLOGY OF RUBBER-TOUGHENED STRUCTURAL EPOXY RESIN SYSTEMS
Introduction
Epoxy Resin Chemistry
Basic Epoxy Chemical Reactions
Kinetics of Cure
Epoxy Reactivity
Modeling of the Cure Process
Rheological Implication of Differences in Reactivity
Modeling Rheological Behavior
Connection between Rheology and Cure
Rheological Studies of Cure
Toughened Epoxy Resins
Carboxy-Terminated Butadiene Acrylonitrile (CTBN)
Polyethersulfone (PES)
Nano Clay Toughening of Epoxy Resins
Toughening with Nano Carbon and Silica Nano Particles
Plasticization
Concluding Comments
Acknowledgments
VISOELASTIC MEASUREMENTS AND PROPERTIES OF RUBBER-MODIFIED EPOXIES
Introduction
State Transitions from Liquid to Solid
Viscoelasticity of Cured Materials
Viscoelastic Behavior Below and Near Gel Point
Liquid-Rubber-Modified Epoxies
Core-Shell Rubber-Modified Epoxies
Ternary Systems with Fillers
Viscoelasticity of Cured Materials
Dynamic Mechanical Study
Dielectric Measurement
Other Remarks
Conclusion
LIGHT, X-RAY, AND NEUTRON SCATTERING TECHNIQUES FOR MISCIBILITY AND PHASE BEHAVIOR STUDIES IN POLYMER BLENDS
Introduction
Brief Theoretical Considerations of Scattering
Light Scattering Experiment
X-ray Scattering
Neutron Scattering
Small-Angle Neutron Scattering (SANS)
Conclusions and Future Outlook
Acknowledgments
MECHANICAL PROPERTIES
Introduction
Morphology and Mechanical Properties of Rubber-Modified Epoxies
Influence of Rubber Concentration
Influence of Initial Cure Temperature
Influence of Curing Agent
Influence of Acrylonitrile Content
Influence of Strain Rate
Kerner Equation
Fracture Toughness
Effect of Concentration on Fracture Toughness
Effect of Strain Rate on Fracture Toughness
Effect of Curing Agent on Fracture Toughness
Conclusion
THERMAL PROPERTIES
Specific Heat
Thermal Conductivity
Main Methods of Characterization
Thermal Steady-State Methods
Thermal Transient Methods
Classical Model to Describe Thermal Conductivity as a Function of Temperature and Degree of Cure
Thermogravimetric Analysis of Rubber/Epoxy Systems
Kinetic Study from TGA
DIELECTRIC PROPERTIES OF ELASTOMERIC MODIFIED EPOXIES
Introduction
Dielectric Study in Rubber/Epoxy Systems
Dielectric Constant
Volume Resistivity (VR)
Conductivity
Combined Studies on Dielectric Constant, Volume Resistivity, and Conductivity
Summary
SPECTROSCOPY ANALYSIS OF MICRO/NANOSTRUCTURED EPOXY/RUBBER BLENDS
Introduction
Fourier Transform Infrared (FTIR) and Raman Spectroscopy
DGEBA Epoxy/Rubber Blends
Other Epoxy/Rubber Blends
FTIR Image and Raman Spectroscopy
Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM)
Acid-Terminated Rubber/DGEBA Epoxy Blends
Hydroxyl-Terminated Rubber/DGEBA Epoxy Blends
Neutral Rubber/DGEBA Epoxy Blends
Other Type Epoxy/Rubber Blends
Other Spectroscopy
Summary
Abbreviations
APPLICATIONS OF TOUGHENED EPOXY RESINS
Introduction
Aerospace Adhesive Applications
Rubber-Modified Resins
Composites
Epoxy Resin Modification
Thermoplastic Modification
Nanoparticle Modification
Other Areas of Application
Thermoset-Based Materials for Optical Applications Containing Azobenzene Choromophores
Introduction
Synthesis and Optical Properties of Cross-linked Azo Polymers
Epoxy-Based Networks
Urethane-Based Networks
Photoaddressable Networks Containing Alkyl Compounds
Conclusions
COMPARISON OF EPOXY/RUBBER BLENDS WITH OTHER TOUGHENING STRATEGIES: THERMOPLASTICS AND HYPERBRANCHED MODIFIERS
Epoxy/Thermoplastic Blends: Development and Properties
Epoxy/Hyperbranched Polymer Blends: Development and Properties
Novel Toughening Approaches for Liquid Molding Technologies
Rubbers as Tougheners: Comparison with Thermoplastics and Hyperbranched Modifiers
Conclusions
RELIABILITY TESTING
Introduction
Reliability Tests Used in Micro/Nanotechnologies
Behavior in Real Applications and Aging Studies of Epoxy/Rubber Blends
Epoxy/Rubber Blends Used in Packaging of Active Electronic Components
Molding Material
Adhesives
Epoxy Matrix Used in Nanocomposites
Conclusions
FAILURE ANALYSIS
Introduction
Methods for Failure Analysis of Epoxy/Rubber Blends
Typical Failure Modes and Failure Mechanisms of Epoxy/Rubber Blends Used in Micro and Nanotechnologies
Mechanical Damages
Fracture
Creep
Ion Contamination
Self Healing
Conclusions
LIFE CYCLE ASSESSMENT (LCA) OF EPOXY-BASED MATERIALS
Introduction to Life Cycle Assessment (LCA)
Significance of Life Cycle Assessment (LCA)
Goal and Scope Definition
Life Cycle Inventory Analysis
Life Cycle Impact Assessment
Life Cycle Result Interpretation
Life Cycle Analysis of Epoxy Systems
Life Cycle Analysis of Epoxy Resins Produced Based on Propylene and Glycerin
Life Cycle Analysis of Epoxy Resin Containing Carbon Nanotubes
Life Cycle Assessment of Wind Turbine Blade Materials
Life Cycle Assessment in Automotive Application
Life Cycle Assessment in Aerospace Application
Life Cycle Assessment of a Novel Hybrid Glass-Hemp/Thermoset Composite
Natural Fiber-Reinforced Epoxy Composites
Conclusion
Index
Centre for Nanoscience and Nanotechnology, Mahatma Gandhi University, Kerala, India. He received his Ph.D. in 1987 in Polymer Engineering from the Indian Institute of Technology (IIT), Kharagpur, India. He is a Fellow of the Royal Society of Chemistry.
Prof. Thomas has (co-)authored more than 600 research papers in international peer-reviewed journals in the area of polymer composites, nanocomposites, membrane separation, polymer blends and alloys, polymeric sca olds for tissue engineering and polymer recycling. Prof. Thomas has been involved in a number of books (35 books), both as author and editor. He has been ranked no. 5 in India with regard to the number of publications (listed in the panel of most productive scientists in the country). He received the coveted Sukumar Maithy Award for the best polymer researcher in the country for the year 2008. The h index of Prof. Thomas is 67 and he has more than 17,000 citations. Prof. Thomas has 4 patents to his credit. Recently he has been awarded CRSI and MRSI awards. Prof. Thomas has supervised 64 PhD theses and has delivered more than 200 invited /plenary and key note talks over 30 countries.
Christophe Sinturel received his Masters degree in Organic Chemistry in 1994 and his Ph.D. in Polymer Science in 1998 from the University Blaise Pascal of Clermont-Ferrand (France). He spent one year at the University of Brighton (UK) in 1999 as Postdoctoral Research Associate before being appointed as an associate professor the same year at the University of Orléans (France). He accepted a full-professor position
at the University of Orléans in 2010. Christophe is currently conducting research in Orléans at the Centre de Recherche sur la Matière Divisée,
a joint research institute of the Centre National de la Recherche Scienti que (CNRS) and the University of Orléans.
His current research interests concern polymer blends, nanostructured polymers, polymer nano-composites and block polymers.
He has published 40 publications in various international journals and books, 2 patents and participated in several international conferences.
Raju Thomas is Vice Chancellor of Middle East University FZE, Ras Al Khaimah, UAE. He received his Ph.D. under the supervision of Prof. abu Thomas, Director of International and Interuniversity Centre for Nanoscience and Nanotechnology, Mahatma Gandhi University, Kottayam,
Kerala, India.
His research works are re ected in his six published research articles in international journals and few articles which are under review status. Also many articles are published in popular journals. He has a wide teaching experience in Chemistry for more than 32 years in Graduate and Postgraduate levels.