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Table of Contents
Intro; Supervisor's Foreword; Abstract; Acknowledgements; Contents; 1 Preamble; References; 2 Introduction; 2.1 Gyroids; 2.1.1 Level Surfaces; 2.1.2 Gyroid Surface; 2.1.3 Single Gyroid; 2.1.4 Double Gyroid; 2.2 Block Copolymer Self-assembly; 2.2.1 Diblock Copolymers; 2.2.2 Triblock Terpolymers; 2.3 Solvent Vapour Annealing; 2.3.1 Diblock Copolymers; 2.3.2 Triblock Copolymers and Terpolymers; 2.3.3 Gyroid-Forming Block Copolymers; 2.4 Block Copolymer Crystallisation; 2.4.1 Spherulites; 2.4.2 Crystallisation Temperature; 2.4.3 Gyroid-Forming Block Copolymers; 2.5 Metamaterials
2.6 Gyroid Optical Metamaterials2.6.1 Fabrication; 2.6.2 Optical Properties; 2.6.3 Simulations and Theoretical Description; References; 3 Methods; 3.1 Terpolymer Thin Films; 3.2 Differential Scanning Calorimetry; 3.3 Annealing; 3.3.1 Thermal Annealing; 3.3.2 In Situ Solvent Vapour Annealing; 3.3.3 Ex Situ Solvent Vapour Annealing; 3.4 Film Thickness Measurements; 3.5 Grazing-Incidence Small- and Wide-Angle X-Ray Scattering; 3.5.1 Paul Scherrer Institute; 3.5.2 Cornell High Energy Synchrotron Source; 3.5.3 Data Analysis; 3.6 Electrodeposition of Gold; 3.7 Optical Characterisation
3.7.1 Optical Microscopy3.7.2 Reflection Goniometry; 3.7.3 Transmission Goniometry; 3.8 Optical Simulations; References; Part I Solvent Vapour Annealing of a Gyroid-Forming Triblock Terpolymer; 4 In Situ GISAXS During Solvent Vapour Annealing of a Gyroid-Forming ISO Triblock Terpolymer; 4.1 Methods; 4.2 Results; 4.2.1 Solvent Vapour Annealing (SVA) Regimes; 4.2.2 Effect of Maximum Swelling Ratio and Solvent Removal Rate; 4.2.3 Effect of Different Solvent and Mixed Solvent Vapours; 4.3 Discussion; 4.3.1 Alternating Gyroid Morphology; 4.3.2 Robust Morphology and Flexible Unit Cell Size
4.4 ConclusionReferences; 5 Preferentially Aligned Crystallisation Within a Single Gyroid Network of an ISO Triblock Terpolymer; 5.1 Methods; 5.2 Results; 5.2.1 Crystalline Superstructure; 5.2.2 Microphase-Separated Morphology; 5.2.3 Correlation of Crystalline Superstructure with Microphase-Separated Morphology; 5.3 Discussion; 5.3.1 Confined Crystallisation; 5.3.2 Multiple Individually Aligned Crystallites; 5.3.3 Crystallite Orientation; 5.3.4 Preferentially Aligned Crystallisation Along the langle111 rangle and langle100 rangle Directions
5.3.5 Distribution of Local Crystallite Orientations5.4 Conclusion; References; Part II Optical Anisotropy in Gyroid Optical Metamaterials; 6 Multi-Domain Gyroid Optical Metamaterials; 6.1 Methods; 6.2 Effective Medium Theories; 6.2.1 Maxwell-Garnett Theory: Spherical Inclusions; 6.2.2 Bruggeman Theory: Spherical Inclusions; 6.2.3 Bruggeman Theory: Ellipsoidal Inclusions; 6.2.4 Model Fitting; 6.3 Results; 6.3.1 Multi-Domain Gyroid Optical Metamaterials; 6.3.2 Effective Medium Models; 6.3.3 Host Refractive Index and Volume Fill Fraction; 6.4 Discussion; 6.4.1 Bruggeman Random Wire Array
2.6 Gyroid Optical Metamaterials2.6.1 Fabrication; 2.6.2 Optical Properties; 2.6.3 Simulations and Theoretical Description; References; 3 Methods; 3.1 Terpolymer Thin Films; 3.2 Differential Scanning Calorimetry; 3.3 Annealing; 3.3.1 Thermal Annealing; 3.3.2 In Situ Solvent Vapour Annealing; 3.3.3 Ex Situ Solvent Vapour Annealing; 3.4 Film Thickness Measurements; 3.5 Grazing-Incidence Small- and Wide-Angle X-Ray Scattering; 3.5.1 Paul Scherrer Institute; 3.5.2 Cornell High Energy Synchrotron Source; 3.5.3 Data Analysis; 3.6 Electrodeposition of Gold; 3.7 Optical Characterisation
3.7.1 Optical Microscopy3.7.2 Reflection Goniometry; 3.7.3 Transmission Goniometry; 3.8 Optical Simulations; References; Part I Solvent Vapour Annealing of a Gyroid-Forming Triblock Terpolymer; 4 In Situ GISAXS During Solvent Vapour Annealing of a Gyroid-Forming ISO Triblock Terpolymer; 4.1 Methods; 4.2 Results; 4.2.1 Solvent Vapour Annealing (SVA) Regimes; 4.2.2 Effect of Maximum Swelling Ratio and Solvent Removal Rate; 4.2.3 Effect of Different Solvent and Mixed Solvent Vapours; 4.3 Discussion; 4.3.1 Alternating Gyroid Morphology; 4.3.2 Robust Morphology and Flexible Unit Cell Size
4.4 ConclusionReferences; 5 Preferentially Aligned Crystallisation Within a Single Gyroid Network of an ISO Triblock Terpolymer; 5.1 Methods; 5.2 Results; 5.2.1 Crystalline Superstructure; 5.2.2 Microphase-Separated Morphology; 5.2.3 Correlation of Crystalline Superstructure with Microphase-Separated Morphology; 5.3 Discussion; 5.3.1 Confined Crystallisation; 5.3.2 Multiple Individually Aligned Crystallites; 5.3.3 Crystallite Orientation; 5.3.4 Preferentially Aligned Crystallisation Along the langle111 rangle and langle100 rangle Directions
5.3.5 Distribution of Local Crystallite Orientations5.4 Conclusion; References; Part II Optical Anisotropy in Gyroid Optical Metamaterials; 6 Multi-Domain Gyroid Optical Metamaterials; 6.1 Methods; 6.2 Effective Medium Theories; 6.2.1 Maxwell-Garnett Theory: Spherical Inclusions; 6.2.2 Bruggeman Theory: Spherical Inclusions; 6.2.3 Bruggeman Theory: Ellipsoidal Inclusions; 6.2.4 Model Fitting; 6.3 Results; 6.3.1 Multi-Domain Gyroid Optical Metamaterials; 6.3.2 Effective Medium Models; 6.3.3 Host Refractive Index and Volume Fill Fraction; 6.4 Discussion; 6.4.1 Bruggeman Random Wire Array