We present an innovative approach to the production of single-crystal iron oxide nanorings employing a solution-based route. Single-crystal hematite (alpha-Fe2O3) nanorings were synthesized using a double anion-assisted hydrothermal method (involving phosphate and sulfate ions), which can be divided into two stages: (1) formation of capsule-shaped alpha-Fe2O3 nanoparticles and (2) preferential dissolution along the long dimension of the elongated nanoparticles (the c axis of alpha-Fe2O3) to form nanorings. The shape of the nanorings is mainly regulated by the adsorption of phosphate ions on faces parallel to c axis of alpha-Fe2O3 during the nanocrystal growth, and the hollow structure is given by the preferential dissolution of the alpha-Fe2O3 along the c axis due to the strong coordination of the sulfate ions. By varying the ratios of phosphate and sulfate ions to ferric ions, we were able to control the size, morphology, and surface architecture to produce a variety of three-dimensional hollow nanostructures. These can then be converted to magnetite (Fe3O4) and maghemite (gamma-Fe2O3) by a reduction or reduction-oxidation process while preserving the same morphology. The structures and magnetic properties of these single-crystal alpha-Fe2O3, Fe3O4, and gamma-Fe2O3 nanorings were characterized by various analytical techniques. Employing off-axis electron holography, we observed the classical single-vortex magnetic state in the thin magnetite nanorings, while the thicker rings displayed an intriguing three-dimensional magnetic configuration. This work provides an easily scaled-up method for preparing tailor-made iron oxide nanorings that could meet the demands of a variety of applications ranging from medicine to magnetoelectronics.
Although it has been known for over 50 years that abnormal concentrations of iron are associated with virtually all neurodegenerative diseases, including Alzheimer's disease, its origin, nature and role have remained a mystery. Here, we use high-resolution transmission electron microscopy (HR-TEM), energy dispersive X-ray (EDX) spectroscopy and electron energy-loss spectroscopy (EELS), electron tomography, and electron diffraction to image and characterize iron-rich plaque core material-a hallmark of Alzheimer's disease pathology-in three dimensions. In these cores, we unequivocally identify biogenic magnetite and/or maghemite as the dominant iron compound. Our results provide an indication that abnormal iron biomineralization processes are likely occurring within the plaque or the surrounding diseased tissue and may play a role in aberrant peptide aggregation. The size distribution of the magnetite cores implies formation from a ferritin precursor, implicating a malfunction of the primary iron storage protein in the brain.
Accurate understanding of the structure of active sites is fundamentally important in predicting catalytic properties of heterogeneous nanocatalysts. We present an accurate determination of both experimental and theoretical atomic structures of surface monatomic steps on industrial platinum nanoparticles. This comparison reveals that the edges of nanoparticles can significantly alter the atomic positions of monatomic steps in their proximity, which can lead to substantial deviations in the catalytic properties compared with the extended surfaces.
Picture perfect: Information about the local topologies of active sites on commercial nanoparticles can be gained with atomic resolution through spherical‐aberration‐corrected transmission electron microscopy (TEM). A powder of Pt nanoparticles on carbon black was examined with two advanced TEM techniques based on recent developments in hardware (aberration correction) and computation (exit wavefunction restoration).
Mössbauer spectra of antiferromagnetic goethite (α-FeOOH) particles usually show an asymmetric line broadening, which increases with increasing temperature, although the magnetic anisotropy is expected to be so large that magnetic relaxation effects should be negligible. By use of high resolution transmission electron microscopy we have studied a sample of goethite particles and have found that the particles contain many defects such as low angle grain boundaries, in accordance with previous studies of other samples of goethite particles. Such defects can result in a magnetic mismatch at the grain boundaries between nanometer-sized grains, leading to a weakened magnetic coupling between the grains. We show that the Mössbauer data of goethite can be explained by fluctuations of the sublattice magnetization directions in such weakly coupled grains. It is likely that the influence of defects such as low angle grain boundaries also plays a role with regards to the magnetic properties in other antiferromagnetic nanograin systems. We discuss the results in relation to Mössbauer studies of α-Fe(2)O(3) and α-Fe(2)O(3)/NiO nanoparticles.
SummaryHigh-angle annular dark-field scanning transmission electron microscopy tomography is applied to the study of Pt and PtCr nanoparticles supported on carbon black, which are used as heterogeneous catalysts in the electrodes of proton exchange membrane fuel cells. By using electron tomography, the three-dimensional architecture of the heterogeneous catalyst system can be determined, providing high-spatial-resolution information about the shapes, faceting and crystallographies of 5-20 nm single and multiply twinned catalyst particles, as well as their positions with respect to the carbon support. Approaches that can be used to provide improved information about the distribution and orientation of the particles on their support are proposed and discussed. Our results show that electron tomography provides important information that is complementary to high-resolution lattice imaging. Both techniques are required to understand fully the nature and role of the surfaces of faceted catalyst particles.
A mechanism of dual enlargement of gold nanoparticles (AuNPs) comprising two steps is described. In the first step, the AuNPs are enlarged by depositing Au atoms on their crystalline faces. In this process, the particles are not only enlarged but they are also observed to multiply: new Au nuclei are formed by the budding and division of the enlarged particles. In the second step, a silver enhancement is subsequently performed by the deposition of silver atoms on the enlarged and newly formed AuNPs to generate bimetallic Au@Ag core-shell structures. The dual nanocatalysis greatly enhances the electron density of the nanostructures, leading to a stronger intensity for colorimetric discrimination as well as better sensitivity for quantitative measurement. Based on this, a simple scanometric assay for the on-slide detection of the food-born pathogen Campylobacter jejuni is developed. After capturing the target bacteria, gold-tagged immunoprobes are added to create a signal on a solid substrate. The signal is then amplified by the dual enlargement process, resulting in a strong color intensity that can easily be recognized by the unaided eye, or measured by an inexpensive flatbed scanner. In this paper, dual nanocatalysis is reported for the first time. It provides a valuable mechanistic insight into the development of a simple and cost-effective detection format.
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