Experimental work has been done to determine changes in the particle shape of portlandite grown in the presence of different ions. To quantify the experimentally observed changes in morphology a new analysis tool was developed, allowing the calculation of the relative surface energies of the crystal facets. The observed morphology in the presence of chlorides and nitrates was facetted particles of a similar shape, the addition of sulfates leads to hexagonal platelet morphology and the addition of silicates leads to the formation of large irregular aggregates. In addition to the experimental work, the surfaces of portlandite were studied with atomistic simulation techniques. The empirical force field used has first been validated. The equilibrium morphology of portlandite in vacuum and in water was then calculated. The results indicate that the presence of water stabilizes the [20.3] surface and changes the morphology. This is consistent with the experimental observation of [20.3] surfaces.
Our work investigates the precipitation mechanism of a seeded calcium carbonate reaction, by using cryogenic TEM to observe the early stages of the reaction. The early precipitation of a hydrated phase is proposed as an intermediate phase before transformation into calcite. Thermodynamic modeling in conjunction with pH, surface potential measurements, and colloidal stability modeling demonstrate that calcite growth is dominated by agglomeration. This is in agreement with the cryogenic TEM observations, which suggest oriented attachment dominates early aggregation. The final stage of the reaction is described by a ripening mechanism that is significantly inhibited when high concentrations of polyacrylic acid (PAA) are used. The different concentrations of PAA lead to significant differences in the final particle substructure observed using cross section TEM. At low PAA concentrations, single crystal particles result, coherent with the proposed early oriented attachment mechanism and interfacial energy calculations. A core shell model is proposed for high PAA concentrations, whereas internal ripening of nanosized pores has been observed for low PAA concentrations, suggesting trapped solvent during the rapid initial particle formation at the relatively high supersaturations (S ) 30) investigated.
The successful scale-out and process intensification using a segmented flow tubular reactor (SFTR) for ultrafine CaCO 3 , BaTiO 3 , and nanosized ZnO from optimized minibatch (20 mL) conditions is presented. The capacity of the SFTR in process intensification was demonstrated by producing ∼ 5 kg batches of BaTiO 3 powders with excellent batch-to-batch reproducibility. The SFTR scale-out or numbering-up capacity was demonstrated for a nanostructured CaCO 3 in 500 g batches by scaling-out from one to six segmented flow tubular reactors run in parallel (scale-out/-up ratio of 5000 compared to lab batch experiments). The SFTR was then used to demonstrate its potential for nanosized ZnO powders producing 50 g lots of these nanopowders in a continuous process, a scale-out/-up ratio of 250 compared to lab batch experiments without any loss of powder quality. The SFTR allows a precise control of precipitation conditions, leading to an excellent reproducibility in powder characteristics, and shows great promise as a simple production process of powders and advanced nanomaterials with highly controlled properties.
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