Standard resin reactivity

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Table of contents

Introduction
Chimie des bismaléimides
Modification par des thermoplastiques
Rupture des bismaléimides
Rupture des matrices modifiées
Rupture des composites
Conclusions
Introduction
Composite materials for aeronautics
Materials
Interesting properties
Limiting properties
Going further with composite materials
Bismaleimide resins
Preamble to the study
1 Bismaleimide resins
1.1 Development of bismaleimide resins
1.1.1 Evolution of the BMI-based thermoset
1.1.2 A whole history of chemical investigation
1.2 Experimental details
1.2.1 Selected materials
1.2.2 Experimental procedures
1.2.2.1 Mixing protocol
1.2.2.2 Spectroscopy
1.2.2.3 Calorimetry
1.2.2.4 Rheological analysis
1.2.2.5 Degradation
1.3 Thermal properties
1.3.1 Thermal degradation
1.3.2 Mechanical properties preservation
1.3.3 Thermomechanical behaviour
1.3.4 Conclusion
1.4 Reactivity
1.4.1 Phenol reactivity
1.4.2 Maleimide/allyl reactivity
1.4.2.1 Alder-ene reaction
1.4.2.2 Addition reactions
1.4.3 Standard resin reactivity
1.5 Kinetics elements
1.5.1 Gelation
1.5.1.1 Theoretical considerations
1.5.1.2 Rheology of bismaleimide resins
1.5.2 Time-Temperature-Transformation diagram
1.5.3 Vitrification
1.6 Network structure
1.6.1 Inhomogeneity in thermosetting polymers
1.6.2 Network architecture analysis
1.6.3 Simulated networks
1.7 Conclusions
2 Morphologies of bismaleimide thermoset and thermoplastics blends
2.1 Phase separation in thermosetting polymers
2.1.1 Flory-Huggins theory
2.1.2 Flory parameter
2.1.3 Reaction-induced phase separation
2.1.3.1 Reactive solvent
2.1.3.2 Pseudo-ternary thermoset
2.2 Literature on bismaleimide/thermoplastic blends
2.2.1 Polyethersulfones
2.2.2 Polyetherimides
2.2.3 Polyesters
2.2.4 Polyimides
2.2.5 Polyether ketones
2.2.6 Other polymers
2.2.7 Conclusion
2.3 Experimental details
2.3.1 Selected materials
2.3.1.1 Thermoset
2.3.1.2 Thermoplastics
2.3.2 Methods
2.3.2.1 Blend preparation
2.3.2.2 In situ temperature controlled microscopy
2.3.2.3 Cured samples preparation
2.3.2.4 Optical microscopy on cured samples
2.3.2.5 Electron Dispersive X-ray Spectroscopy
2.3.2.6 Dynamic Mechanical Analysis
2.3.2.7 Rheology
2.4 Phase separation in bismaleimide/solubilised thermoplastic blends
2.4.1 Phase separation behaviours
2.4.1.1 Polyetherimide
2.4.1.2 Polyethersulfone
2.4.2 Final morphologies
2.4.2.1 Influence of curing conditions
2.4.2.2 Comparison between thermoplastics
2.4.2.3 Deeper look on morphologies
2.4.3 Thermomechanical analysis
2.4.4 First conclusions on solubilised thermoplastics
2.5 Bismaleimide/thermoplastic particles blends
2.5.1 Soluble particles
2.5.1.1 Experimental considerations
2.5.1.2 Influence of the curing conditions
2.5.1.3 Conclusion on morphological control
2.5.2 Non-soluble particles
2.6 Conclusion
3 Fracture of bismaleimide resins
3.1 Polymer fracture
3.1.1 Fracture mechanics
3.1.1.1 Linear elastic fracture mechanics
3.1.1.2 Crack propagation
3.1.1.3 Fracture modes
3.1.1.4 Stress limitation at a crack-tip
3.1.2 Failure of thermosets
3.1.3 Crack propagation in glassy polymers
3.2 Experimental details
3.2.1 Materials
3.2.2 Methods
3.2.2.1 Mechanical characterisation
3.2.2.2 Compact tension
3.2.2.3 Double Cantilever Drilled Compression
3.2.2.4 Optical Imaging
3.2.2.5 Interferometry
3.2.2.6 Atomic force microscopy
3.2.2.7 SEM Fractography
3.3 Neat bismaleimide network fracture
3.3.1 Mechanical properties
3.3.1.1 Uniaxial tension
3.3.1.2 Uniaxial compression
3.3.1.3 Extrapolated microscopic behaviour
3.3.1.4 Molecular behaviour
3.3.2 Failure at the macroscopic scale
3.3.3 Crack propagation kinetics
3.3.3.1 Evaluation of the stress intensity factor
3.3.3.2 Considerations on the crack opening measurement
3.3.3.3 Velocity measurements and K(v) curves
3.4 Influence of the network architecture
3.4.1 Non-monotonic crack propagation
3.4.2 Network modification
3.5 Modelling toughness
3.5.1 Steady state toughness
3.5.2 Material behaviour at the crack-tip
3.5.3 Steady state crack propagation
3.6 Conclusion
4 Fracture in heterogeneous materials
4.1 Material toughness
4.1.1 Toughening of thermosetting polymers
4.1.1.1 Modifiers for thermosets
4.1.1.2 Toughening mechanisms
4.1.2 Toughness in composite laminates
4.2 Experimental details
4.2.1 Materials
4.2.1.1 Modified resins
4.2.1.2 Composites
4.2.2 Methods
4.2.2.1 Tension
4.2.2.2 Compact tension
4.2.2.3 Double Cantilever Drilled Compression
4.2.2.4 Composite delamination
4.2.2.5 Atomic force microscopy
4.2.2.6 Fractography
4.3 Fracture behaviour in matrices
4.3.1 Mechanical properties
4.3.2 Toughening
4.3.3 Crack path in modified matrices
4.3.3.1 Particles from phase separation
4.3.3.2 Initially insoluble particles
4.3.4 Conclusions
4.4 Composite materials properties
4.4.1 Selected formulations
4.4.2 Morphologies
4.4.2.1 Neat bismaleimide-based composite
4.4.2.2 Polyethersulfone-modified composite
4.4.2.3 Polyamide-imide-modified composite
4.4.2.4 PES/PAI-modified composite
4.4.2.5 Conclusions
4.4.3 Toughening
4.4.4 Crack path
4.4.4.1 Neat bismaleimide-based composite
4.4.4.2 Polyethersulfone-modified composite
4.4.4.3 Polyamide-imide-modified composite
4.4.4.4 PES/PAI-modified composite
4.4.4.5 Matrix-composite comparison
4.5 Conclusions
4.5.1 On crack propagation in modified resins
4.5.2 On composite processing and toughening
5 Suggestions for further work and general conclusion
5.1 Reactivity of bismaleimides
5.1.1 Chemical characterisations
5.1.2 Simulated network architecture
5.2 Fracture mechanics of bismaleimides
5.3 Failure of modified resins
5.4 Composites properties
5.4.1 Fracture of composites
5.4.2 Compression after impact
5.4.3 Other types of alteration
5.5 Conclusions
Abbreviations
Bibliography
Appendix A: NMR spectra
Appendix B: Modulus loss calculation
Appendix C: Epoxy TTT diagram
Appendix D: Simulation program
Appendix E: Solubility parameters
Appendix F: Thermoplastics TGA
Appendix G: Edge detection tools