Tailoring the solution chemistry of metal halide perovskites requires a detailed understanding of precursor aggregation and coordination. In this work, we use various scattering techniques, including dynamic light scattering (DLS), small angle neutron scattering (SANS), and spin-echo SANS (SESANS) to probe the nanostructures from 1 nm to 10 μm within two different lead-halide perovskite solution inks (MAPbI ₃and a triple-cation mixed-halide perovskite). We find that DLS can misrepresent the size distribution of the colloidal dispersion and use SANS/SESANS to confirm that these perovskite solutions are mostly comprised of 1-2 nm-sized particles. We further conclude that if there are larger colloids present, their concentration must be <0.005% of the total dispersion volume. With SANS, we apply a simple fitting model for two component microemulsions (Teubner-Strey), demonstrating this as a potential method to investigate the structure, chemical composition, and colloidal stability of perovskite solutions, and we here show that MAPbI ₃solutions age more drastically than triple cation solutions.

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The impact of the additive 1,8-diiodooctane on the morphology of bulk-heterojunction solar cells based on the systems P3HT:PC₇₁BM, PTB7:PC₇₁BM and PTB7-Th:PC₇₁BM is studied using a combination of Small Angle Neutron Scattering (SANS) and Atomic Force Microscopy (AFM). The results clearly show that while in the P3HT:PC₇₁BM system, the additive DIO promotes a slight coarsening of the phase domains (type I additive), in the systems PTB7:PC₇₁BM and PTB7-Th:PC₇₁BM, DIO promotes a large decrease in the size of the phase domains (type II additive). SANS is demonstrated as being particularly useful at detecting the minor morphological changes observed in the P3HT:PC₇₁BM system, which can be hardly seen in AFM. This work illustrates how SANS complements AFM and both techniques when used together provide a deeper insight into the nanoscale structure in thin organic photovoltaic (OPV) device films.

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We investigate the morphological development of polystyrene (PS)-C ₆₀ nanocomposites along the length of a prototype co-rotating twin-screw extruder with sampling capabilities. The effects of C ₆₀ concentration and output on the morphological evolution along the extruder are studied employing a suite of characterization techniques covering a wide range of length-scales, thereby shedding new light on the dispersion mechanism in this model system. We show that the relatively new spin-echo small-angle neutron scattering (SESANS) technique is well suited to probe both the distribution and the dispersion of C ₆₀ . SESANS complements optical microscopy (OM) data as it covers sampling areas several orders of magnitude larger than OM. The multi-scale morphological information conveyed by OM, SESANS, SANS and rheological data shows that for larger outputs, C ₆₀ agglomerates are eroded as they travel along the extruder, resulting in C ₆₀ dispersion and distribution at both molecular and micrometric levels. The picture is more complex when smaller feed rates are used, as the evolution of C ₆₀ dispersion depends on the C ₆₀ loading. For larger C ₆₀ contents, agglomeration develops along the extruder, whereas dispersion is improved for smaller C ₆₀ contents. Overall, it is concluded that an over-high feed rate in extrusion does not necessarily result in a bigger size of the nanoparticle agglomerates because of the complex interplay between stresses and residence time.

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We investigated the effect of the feeding formulation (premixed powders of pure components versus solvent-blended mixture) of polystyrene–C60 composites on the dispersion and reagglomeration phenomena developing along the barrel of a twin-screw extruder. The dispersion of C60 in the PS matrix is studied over different length scales using a combination of optical microscopy, spin-echo small-angle neutron scattering (SESANS), small-angle neutron scattering (SANS), small-angle X-ray scattering (SAXS), and wide-angle X-ray scattering (WAXS). When a solvent-blended mixture is used as the feeding formulation, the inlet material contains essentially molecularly dispersed C60 as revealed by the nanodomains with very small phase contrast. However, C60 reagglomeration occurs along the extruder, creating a morphology still containing only nanodomains but with much higher phase contrast. In the case of mixed powders, the material evolves from the initial macroscopic mixture of pure polystyrene and C60 into a composite simultaneously containing micro- and nanoaggregates of C60 as well as C60 molecularly dispersed in the matrix. Our results show that the two different initial feeding formulations with widely different initial morphologies converge along the extruder, through opposite morphological pathways, into a similar final nanomorphology which is dictated by the interplay between the thermodynamics of the system and the flow. Correlations between the morphological evolution along the extruder and the thermorheological properties of the composites are identified.@en