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Structural rearrangement of polystyrene colloidal crystals under drysintering conditions has been revealed by in situ grazing incidence X-rayscattering. Measured diffraction patterns were analysed using distorted waveBorn approximation (DWBA) theory and the structural parameters of as-growncolloidal crystals of three different particle sizes were determined forin-plane and out-of-plane directions in a film. By analysing the temperatureevolution of diffraction peak positions, integrated intensities, and widths thedetailed scenario of structural rearrangement of crystalline domains at ananoscale has been revealed, including thermal expansion, particle shapetransformation and crystal amorphisation. Based on DWBA analysis we demonstratethat in the process of dry sintering the shape of colloidal particles in acrystal transforms from a sphere to a polyhedron. Our results deepen theunderstanding of thermal annealing of polymer colloidal crystals as anefficient route to the design of new nano-materials.

Unravelling structural rearrangement of polymer colloidal crystals under dry sintering conditions