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This thesis presents an in-depth study on the effect of colloidal particle shape and formation mechanism on self-organization and the final crystal symmetries that can be achieved. It demonstrates how state-of-the-art X-ray diffraction techniques can be used to produce detailed characterizations of colloidal crystal structures prepared using different self-assembly techniques, and how smart systems can be used to investigate defect formation and diffusion in-situ. One of the most remarkable phenomena exhibited by concentrated suspensions of colloidal particles is the spontaneous self-organization into structures with long-range spatial and/or orientational orders. The study also reveals the subtle structural variations that arise by changing the particle shape from spherical to that of a rounded cube. In particular, the roundness of the cube corners, when combined with the self-organization pathway, convective assembly or sedimentation, was shown to influence the final crystal symmetries.

Physics. --- Soft and Granular Matter, Complex Fluids and Microfluidics. --- Physical Chemistry. --- Characterization and Evaluation of Materials. --- Surfaces and Interfaces, Thin Films. --- Chemistry, Physical organic. --- Surfaces (Physics). --- Physique --- Surfaces (Physique) --- Physics --- Physical Sciences & Mathematics --- Atomic Physics --- Colloidal crystals. --- Colloids. --- Dispersoids --- Gels --- Hydrogels --- Sols --- Crystals, Colloidal --- Physical chemistry. --- Amorphous substances. --- Complex fluids. --- Materials science. --- Materials --- Thin films. --- Surfaces. --- Amorphous substances --- Chemistry, Physical and theoretical --- Diffusion --- Matter --- Micelles --- Particles --- Rheology --- Solution (Chemistry) --- Surface chemistry --- Colloids --- Properties --- Surfaces (Technology) --- Chemistry, Physical organic --- Chemistry, Organic --- Materials—Surfaces. --- Films, Thin --- Solid film --- Solid state electronics --- Solids --- Coatings --- Thick films --- Material science --- Physical sciences --- Chemistry, Theoretical --- Physical chemistry --- Theoretical chemistry --- Chemistry --- Complex liquids --- Fluids, Complex --- Liquids --- Soft condensed matter