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Abstract: The photocatalytic (PC) performance of titanium dioxide (TiO2) nanoparticles strongly depends on their specific surface, the presence of crystal defects, their crystal phase, and the exposed crystal facets. In order to understand which of these factors contributes most significantly to the PC activity of TiO2 colloids, all of them have to be individually analyzed. This study entails the synthesis of five anatase nanocrystal samples. By maintaining the same reactant ratios as well as hydrothermal sol–gel synthesis route and only varying the autoclaving time or temperature, different crystallite sizes are obtained under comparable experimental conditions. A decrease in PC performance with increase in specific surface area is found. Such an unexpected counterintuitive result establishes the basis for a better understanding of the crucial factors that ultimately determine the PC activity. These are investigated by studying nanocrystals bulk and surface structure and morphology using a selection of complementary analysis methods (X‐ray photoelectron spectroscopy (XPS), X‐ray absorption fine structure (XAFS), X‐ray diffraction (XRD)…). It is found that a change in the nanocrystal morphology from an equilibrium state truncated tetragonal bipyramid to a more elongated rod‐like structure accompanied by an increase in oxygen vacancies is responsible for an augmented PC activity of the TiO2 nanocrystals. [ABSTRACT FROM AUTHOR]

To tailor superparamagnetic iron oxide nanoparticles (SPIONs) to the specific needs of diverse application fields, it is essential to understand not only their intrinsic properties but also their interactions with each other. Theoretical models predicting/explaining the magnetization behavior of macroscopic samples containing millions of SPIONs are intricate due to the complexity of the underlying relaxation mechanisms in alternating fields. This study introduces supraparticles (SPs) as model architectures to empirically investigate magnetic interactions within and between large SPION clusters (>100 nanoparticles (NPs)). For this purpose, NP dispersions containing SPIONs and silica (SiO2)NPs as non‐magnetic building blocks are spray‐dried to form binary SPs. Selective salt‐induced agglomeration of the two building block types before spray‐drying is utilized to tailor SP architectures, including control over SPION cluster size, shape, and proximity. Magnetic particle spectroscopy (MPS), operating under ambient conditions, reveals altered magnetization behavior for different cluster structures. Not only the nearest SPION neighbors, but the whole cluster structure up to several micrometers is decisive for the magnetization behavior. This highlights the importance of long‐range magnetic interactions. This work presents a versatile approach for designing model architectures to advance empirical interaction studies between SPIONs in macroscopic samples. [ABSTRACT FROM AUTHOR]