It is demonstrated that Bragg coherent diffraction imaging can be used to visualize dislocation propagation in three dimensions during the repeated growth and dissolution of calcite crystals. Atomic-level defects such as dislocations play key roles in determining the macroscopic properties of crystalline materials1,2. Their effects range from increased chemical reactivity3,4 to enhanced mechanical properties5,6. Dislocations have been widely studied using traditional techniques such as X-ray diffraction and optical imaging. Recent advances have enabled atomic force microscopy to study single dislocations7 in two dimensions, while transmission electron microscopy (TEM) can now visualize strain fields in three dimensions with near-atomic resolution8,9,10. However, these techniques cannot offer three-dimensional imaging of the formation or movement of dislocations during dynamic processes. Here, we describe how Bragg coherent diffraction imaging (BCDI; refs 11, 12) can be used to visualize in three dimensions, the entire network of dislocations present within an individual calcite crystal during repeated growth and dissolution cycles. These investigations demonstrate the potential of BCDI for studying the mechanisms underlying the response of crystalline materials to external stimuli.

The term mesocrystal has been widely used to describe crystals that form by oriented assembly, and that exhibit nanoparticle substructures. Using calcite crystals co-precipitated with polymers as a suitable test case, this article looks critically at the concept of mesocrystals. Here we demonstrate that the data commonly used to assign mesocrystal structure may be frequently misinterpreted, and that these calcite/polymer crystals do not have nanoparticle substructures. Although morphologies suggest the presence of nanoparticles, these are only present on the crystal surface. High surface areas are only recorded for crystals freshly removed from solution and are again attributed to a thin shell of nanoparticles on a solid calcite core. Line broadening in powder X-ray diffraction spectra is due to lattice strain only, precluding the existence of a nanoparticle sub-structure. Finally, study of the formation mechanism provides no evidence for crystalline precursor particles. A re-evaluation of existing literature on some mesocrystals may therefore be required.

Bacterial magnetosomes (MS) are well-defined membrane-enveloped single-domain iron oxide (magnetite) nanoparticles, which are susceptible to genetic and chemical engineering. Additionally, the possibility to manipulate these particles by external magnetic fields facilitates their application in biomedicine and biotechnology, e.g. as magnetic resonance imaging probes or for drug delivery purposes. However, current purification protocols are poorly characterized, thereby hampering standardized and reproducible magnetosome production and thus, reliable testing for in vivo applications. In that context, the establishment of reproducible particle isolation procedures as well as the identification of high quality control parameters and the evaluation of potential cytotoxic effects of purified particles are of major importance. In this study, we characterize a multi-step purification protocol for MS with regard to purity, iron content, size and polydispersity of magnetite particles. In addition, we address potential cytotoxic effects of isolated MS when incubated with mammalian cells. Overall, we provide a detailed overview of the process-structure relationship during the isolation of MS and thus, identify prerequisites for high-yield MS production and their future application in the biomedical and biotechnological field. STATEMENT OF SIGNIFICANCE: Magnetic nanoparticles are of increasing interest for a variety of biomedical and biotechnological applications. Due to their unprecedented material characteristics, bacterial magnetosomes represent a promising alternative to chemically synthesized iron oxide nanoparticles. As applications require well-defined, highly purified and fully characterized nanoparticles, reliable protocols are necessary for efficient and reproducible magnetosome isolation. In our study, we evaluate an improved magnetosome extraction procedure and monitor quality parameters such as particle size distribution, membrane integrity and purity of the suspension by a combination of physicochemical and biochemical methods. Furthermore, the cytotoxicity of the isolated magnetosomes is assessed using different cell lines. In summary, our study helps to establish prerequisites for many real-world applications of magnetosomes in the field of biotechnology and biomedicine.