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In situ and ex situ SAXS investigation of colloidal sedimentation onto laterally patterned support
(2009)
We report on in situ investigations of colloidal ordering during gravity sedimentation from a colloidal suspension onto a prepatterned support using a polymeric surface relief grating (SRG) as the support. The ordering of colloids with a diameter of 420 nm was investigated by means of grazing-incidence small-angle X-ray scattering (GISAXS) and transmission SAXS using a preparation cell guaranteeing stable temperature and humidity. GISAXS was used for in situ monitoring of the time evolution of colloidal ordering within the whole illuminated sample area. The onset of ordering was indicated by the increase of integrated intensity within a small time frame shortly before complete evaporation of the dispersant. Single domains of coated samples were investigated ex situ by SAXS in transmission geometry where the irradiated sample area was 200 x 200 mu m(2) only. Domains with the typical size of a few millimeters were observed varying in orientation and crystallographic structure for various positions at the sample. They were mainly oriented along the grooves of the grating, confirming the influence of the underlying grating on colloidal ordering.
Structuring overmany length scales is a design strategy widely used in Nature to create materials with unique functional properties. We here present a comprehensive analysis of an adult sea urchin spine, and in revealing a complex, hierarchical structure, showhow Nature fabricates a material which diffracts as a single crystal of calcite and yet fractures as a glassy material. Each spine comprises a highly oriented array of Mg-calcite nanocrystals in which amorphous regions and macromolecules are embedded. It is postulated that this mesocrystalline structure forms via the crystallization of a dense array of amorphous calcium carbonate (ACC) precursor particles. A residual surface layer of ACC and/or macromolecules remains around the nanoparticle units which creates the mesocrystal structure and contributes to the conchoidal fracture behavior. Nature's demonstration of howcrystallization of an amorphous precursor phase can create a crystalline material with remarkable properties therefore provides inspiration for a novel approach to the design and synthesis of synthetic composite materials.