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Table of contents
Chapter 1: From polymer physics to the toughening of hydrogels
1.1. Polymer network physics
1.2. Fracture of soft matter
1.2.1. “Bulk” vision of fracture
1.2.2. Molecular vision
1.3. Reinforcement of hydrogels
1.3.1. Homogeneous networks
1.3.2. Introducing an energy dissipation mechanism
1.4. Using dynamic coordination crosslinks
1.4.1. Transient networks with versatile dynamics
1.4.2. Toughened gels
1.5. Objectives of this project
Chapter 2: Preparation and microstructure of a dual-crosslink hydrogel
2.1. Gel synthesis
2.1.1. Synthesis of the P(AAm-co-VIm) chemical gel
2.1.2. Synthesis of the P(AAm-co-VIm)/Ni2+ dual crosslink gels
2.2. Absorption of Ni2+ ions
2.2.1. Absorption kinetics of Ni2+ ions
2.2.2. Influence of [NaCl]
2.2.3. Absorption isotherms – influence of [Ni2+]
2.3. Stress-free dynamics – study by dynamic light scattering (DLS)
2.3.1. Dynamic Light Scattering – Principles and protocol
2.3.2. Results for a bare chemical gel
2.3.3. Results for a “One-pot” dual-crosslink gel
2.3.4. Conclusions
2.4. Linear mechanical behavior at small deformations
2.4.1. Rheology of a chemical gel
2.4.2. Rheology of a “One-Pot” dual-crosslink hydrogel
2.4.3. Comparing “One-pot” and “Diffusion” dual-crosslink hydrogels
2.4.4. Fitting with fractional model
2.4.5. Relaxation experiments
2.4.6. Conclusions
2.5. Small-Angle X-Ray scattering experiments
2.5.1. SAXS – Principle and protocol
2.5.2. Qualitative analysis
2.5.3. Attempt at quantitative analysis
2.5.4. Conclusions from X-ray scattering
2.6. Conclusion on microstructure and dynamics
Chapter 3 : Large deformations of a dual-crosslink hydrogels with Ni2+ ions
3.1. Standard uniaxial tensile tests: continuous loading
3.1.1. Comparison of “One-pot” and “Diffusion” gels with [Ni2+] = 100 mmol/L
3.1.2. Continuous loading
3.1.3. Discussion
3.2. Cyclic testing
3.2.1. Influence of stretch and stretch-rate
3.2.2. Damage during cycles?
3.3. Relaxation
3.4. Fracture of Ni2+ dual-crosslink hydrogels
3.4.1. Single-notch fracture under continuous stretching
3.4.2. Delayed fracture of “pure-shear” samples
3.5. Conclusions and discussions
Chapter 4: Dual-crosslink hydrogels with fast dynamics
4.1. Preparation
4.1.1. Cu2+ dual-crosslink hydrogel
4.1.2. Zn2+ dual-crosslink hydrogels
4.1.3. Absorption isotherms
4.2. Rheology
4.2.1. Cu2+ and Zn2+ dual-crosslink hydrogels
4.2.2. Zn2+ dual-crosslink hydrogel – “One-pot” vs. “Diffusion”
4.3. Small-angle X-Ray scattering
4.3.1. General observations
4.3.2. Fitting
4.3.3. Scattered intensity normalization method
4.3.4. Normalized results – comparison between Ni2+ and Zn2+ dual-crosslink hydrogels
4.3.5. Conclusions
4.4. Large deformations
4.4.1. “One-Pot” vs “Diffusion” Zn2+ hydrogels
4.4.2. Tensile tests on Zn2+ and Cu2+ dual-crosslink hydrogels
4.5. Cyclic tests
4.5.1. Influence of stretch-rate and stretch
4.5.2. Damage during cycles?
4.6. Fracture of a fast dual-crosslink hydrogel
4.6.1. Single-notch fracture under continuous stretching
4.6.2. Delayed fracture of “pure-shear” samples of Zn2+ dual-crosslinked hydrogel
4.7. Conclusions
Chapter 5: Slowing down the dynamics
5.1. P(AAm-co-VIm) – Hg2+ hydrogels
5.1.1. Preparation and absorption isotherms
5.1.2. Linear rheology
5.1.3. Small angle X-Ray scattering
5.1.4. Tensile tests
5.1.5. Conclusions on P(AAm-co-VIm)-Hg2+ dual-crosslink hydrogel
5.2. Synthesis of P(AAm-co-tPy) hydrogels
5.3. Rheology of the P(AAm-co-tPy) chemical hydrogel
5.4. Incorporation of physical bonds
5.5. Rheology of the slow Terpyridine-Zn2+ hydrogel
5.6. Behavior in large deformations
5.6.1. Tensile tests
5.6.2. Cycles
5.6.3. Fracture – Single notch test
5.7. Discussion and conclusions
Chapter 6: One bond to rule them all
6.1. Linear rheology
6.2. Large deformations
6.2.1. Tensile tests
6.2.2. Cyclic
6.3. General remarks on the results in large deformations
6.4. Fracture
6.4.1. Single edge notch
6.4.2. Delayed fracture of pure shear samples
6.5. On the dynamic behavior of the dual-crosslink network
Chapter 7: Mapping the damage in dual-crosslink hydrogels with mechanophores
7.1. Mechanophores in hydrogels
7.2. A hydrosoluble dioxetane derivative to obtain time-resolved fracture information
7.2.1. Synthesis of the mechanophore and the hydrogel
7.2.2. Results and discussion
7.3. Anthracene Diels-Alder adduct as a crosslinker
7.3.1. Synthesis of the mechanophore
7.3.2. Synthesis of the chemical network with mechanophore
7.3.3. Mechanical properties of the dual-crosslinked hydrogel with mechanophores
7.3.4. Imaging the fracture front
7.4. Conclusion and perspectives
